# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013
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#
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# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
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# fide research purposes only. It may contain copyright material
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data_inp1bar1
#TrackingRef 'Khuong1_Deposition_04May12.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C30 H35 N5 Rh, C24 H20 B'
_chemical_formula_sum 'C54 H55 B N5 Rh'
_chemical_formula_weight 887.75
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Triclinic
_symmetry_space_group_name_H-M P-1
_symmetry_space_group_name_Hall '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 10.8373(3)
_cell_length_b 15.3768(4)
_cell_length_c 15.4028(5)
_cell_angle_alpha 113.222(2)
_cell_angle_beta 90.9210(10)
_cell_angle_gamma 102.2110(10)
_cell_volume 2291.27(11)
_cell_formula_units_Z 2
_cell_measurement_temperature 150(2)
_cell_measurement_reflns_used 9981
_cell_measurement_theta_min 2.356
_cell_measurement_theta_max 26.269
_exptl_crystal_description Plates
_exptl_crystal_colour Yellow
_exptl_crystal_size_max 0.32
_exptl_crystal_size_mid 0.14
_exptl_crystal_size_min 0.09
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.287
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 928
_exptl_absorpt_coefficient_mu 0.415
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.8781
_exptl_absorpt_correction_T_max 0.9632
_exptl_absorpt_process_details 'SADABS (Bruker, 2001)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 150(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker kappa APEXII CCD Diffractometer'
_diffrn_measurement_method '\f scans, and \w scans with \k offsets'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 32636
_diffrn_reflns_av_R_equivalents 0.0464
_diffrn_reflns_av_sigmaI/netI 0.0414
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_theta_min 2.36
_diffrn_reflns_theta_max 25.00
_reflns_number_total 7984
_reflns_number_gt 7058
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2007)'
_computing_cell_refinement 'APEX2 (Bruker, 2007)'
_computing_data_reduction 'APEX2 (Bruker, 2007)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0285P)^2^+1.7459P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 7984
_refine_ls_number_parameters 553
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0375
_refine_ls_R_factor_gt 0.0311
_refine_ls_wR_factor_ref 0.0768
_refine_ls_wR_factor_gt 0.0729
_refine_ls_goodness_of_fit_ref 1.037
_refine_ls_restrained_S_all 1.037
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.777238(17) 0.686315(12) 0.625338(13) 0.01982(7) Uani 1 1 d . . .
N1 N 0.82312(17) 0.90680(13) 0.76885(13) 0.0203(4) Uani 1 1 d . . .
C2 C 0.7682(2) 0.81038(16) 0.73987(16) 0.0211(5) Uani 1 1 d . . .
N3 N 0.70232(18) 0.80715(13) 0.81315(14) 0.0235(4) Uani 1 1 d . . .
C4 C 0.7158(2) 0.89828(17) 0.88524(17) 0.0274(5) Uani 1 1 d . . .
H4 H 0.6781 0.9135 0.9431 0.033 Uiso 1 1 calc R . .
C5 C 0.7919(2) 0.96097(17) 0.85796(17) 0.0262(5) Uani 1 1 d . . .
H5 H 0.8195 1.0295 0.8928 0.031 Uiso 1 1 calc R . .
N1' N 0.80176(19) 0.53274(15) 0.79266(15) 0.0297(5) Uani 1 1 d . . .
N2' N 0.83691(18) 0.55531(14) 0.71973(15) 0.0270(5) Uani 1 1 d . . .
N3' N 0.77889(17) 0.62369(13) 0.72312(14) 0.0230(4) Uani 1 1 d . . .
C4' C 0.7078(2) 0.64404(17) 0.79716(17) 0.0248(5) Uani 1 1 d . . .
C5' C 0.7223(2) 0.58545(18) 0.84210(18) 0.0309(6) Uani 1 1 d . . .
H5' H 0.6845 0.5826 0.8964 0.037 Uiso 1 1 calc R . .
C6 C 0.9157(2) 0.94821(15) 0.72106(16) 0.0192(5) Uani 1 1 d . . .
C7 C 1.0380(2) 0.93299(16) 0.72483(16) 0.0224(5) Uani 1 1 d . . .
C8 C 1.1267(2) 0.97478(17) 0.68015(17) 0.0267(5) Uani 1 1 d . . .
H9 H 1.2095 0.9633 0.6795 0.032 Uiso 1 1 calc R . .
C9 C 1.0987(2) 1.03300(18) 0.63621(17) 0.0304(6) Uani 1 1 d . . .
C10 C 0.9763(2) 1.04584(17) 0.63475(18) 0.0300(6) Uani 1 1 d . . .
H11 H 0.9559 1.0849 0.6045 0.036 Uiso 1 1 calc R . .
C11 C 0.8821(2) 1.00366(16) 0.67601(17) 0.0243(5) Uani 1 1 d . . .
C12 C 1.0725(2) 0.87615(19) 0.7773(2) 0.0325(6) Uani 1 1 d . . .
H13A H 1.0286 0.8074 0.7436 0.049 Uiso 1 1 calc R . .
H13B H 1.0471 0.9016 0.8417 0.049 Uiso 1 1 calc R . .
H13C H 1.1646 0.8823 0.7810 0.049 Uiso 1 1 calc R . .
C13 C 1.2014(3) 1.0843(2) 0.5962(2) 0.0492(8) Uani 1 1 d . . .
H14A H 1.1635 1.0937 0.5433 0.074 Uiso 1 1 calc R . .
H14B H 1.2635 1.0447 0.5733 0.074 Uiso 1 1 calc R . .
H14C H 1.2438 1.1478 0.6459 0.074 Uiso 1 1 calc R . .
C14 C 0.7495(2) 1.01838(19) 0.6726(2) 0.0349(6) Uani 1 1 d . . .
H15A H 0.7432 1.0562 0.6349 0.052 Uiso 1 1 calc R . .
H15B H 0.7302 1.0537 0.7373 0.052 Uiso 1 1 calc R . .
H15C H 0.6889 0.9549 0.6433 0.052 Uiso 1 1 calc R . .
C6' C 0.8399(3) 0.4504(2) 0.8025(2) 0.0381(7) Uani 1 1 d . . .
H16A H 0.8398 0.4586 0.8696 0.046 Uiso 1 1 calc R . .
H16B H 0.9272 0.4495 0.7849 0.046 Uiso 1 1 calc R . .
C7' C 0.7504(2) 0.35569(19) 0.73979(19) 0.0308(6) Uani 1 1 d . . .
C8' C 0.7701(3) 0.3051(2) 0.6466(2) 0.0527(9) Uani 1 1 d . . .
H22 H 0.8433 0.3292 0.6222 0.063 Uiso 1 1 calc R . .
C9' C 0.6840(4) 0.2195(2) 0.5881(2) 0.0605(10) Uani 1 1 d . . .
H9' H 0.6984 0.1854 0.5241 0.073 Uiso 1 1 calc R . .
C10' C 0.5783(3) 0.1844(2) 0.6229(3) 0.0551(9) Uani 1 1 d . . .
H10' H 0.5189 0.1262 0.5830 0.066 Uiso 1 1 calc R . .
C11' C 0.5586(3) 0.2328(2) 0.7148(3) 0.0530(8) Uani 1 1 d . . .
H11' H 0.4862 0.2077 0.7392 0.064 Uiso 1 1 calc R . .
C12' C 0.6434(3) 0.3182(2) 0.7727(2) 0.0412(7) Uani 1 1 d . . .
H18 H 0.6277 0.3518 0.8364 0.049 Uiso 1 1 calc R . .
C1A C 0.6283(2) 0.71594(17) 0.81428(19) 0.0289(6) Uani 1 1 d . . .
H1A H 0.5549 0.6882 0.7645 0.035 Uiso 1 1 calc R . .
H1B H 0.5951 0.7295 0.8766 0.035 Uiso 1 1 calc R . .
C1B C 0.6781(2) 0.72427(18) 0.52981(17) 0.0278(5) Uani 1 1 d . . .
H1B1 H 0.6474 0.7686 0.5825 0.033 Uiso 1 1 calc R . .
C2B C 0.8067(2) 0.74768(17) 0.52134(17) 0.0263(5) Uani 1 1 d . . .
H2B H 0.8580 0.8042 0.5706 0.032 Uiso 1 1 calc R . .
C3B C 0.8714(2) 0.68948(18) 0.43910(18) 0.0307(6) Uani 1 1 d . . .
H3B1 H 0.9401 0.7347 0.4257 0.037 Uiso 1 1 calc R . .
H3B2 H 0.8089 0.6549 0.3817 0.037 Uiso 1 1 calc R . .
C4B C 0.9276(2) 0.61502(18) 0.45939(18) 0.0311(6) Uani 1 1 d . . .
H4B1 H 0.9347 0.5620 0.3983 0.037 Uiso 1 1 calc R . .
H4B2 H 1.0143 0.6472 0.4929 0.037 Uiso 1 1 calc R . .
C5B C 0.8490(2) 0.57163(16) 0.51879(17) 0.0260(5) Uani 1 1 d . . .
H5B H 0.8936 0.5648 0.5685 0.031 Uiso 1 1 calc R . .
C6B C 0.7188(2) 0.54099(16) 0.50780(17) 0.0271(5) Uani 1 1 d . . .
H6B H 0.6811 0.5176 0.5521 0.033 Uiso 1 1 calc R . .
C7B C 0.6309(2) 0.54140(18) 0.43103(18) 0.0334(6) Uani 1 1 d . . .
H7B1 H 0.5574 0.4846 0.4125 0.040 Uiso 1 1 calc R . .
H7B2 H 0.6764 0.5346 0.3744 0.040 Uiso 1 1 calc R . .
C8B C 0.5825(2) 0.63487(19) 0.4630(2) 0.0356(6) Uani 1 1 d . . .
H8B1 H 0.5585 0.6452 0.4062 0.043 Uiso 1 1 calc R . .
H8B2 H 0.5050 0.6262 0.4948 0.043 Uiso 1 1 calc R . .
B1C B 0.2716(2) 0.70406(18) 0.92656(18) 0.0190(5) Uani 1 1 d . . .
C11C C 0.4034(2) 0.76583(16) 0.99757(16) 0.0195(5) Uani 1 1 d . . .
C12C C 0.4939(2) 0.72461(18) 1.02196(17) 0.0260(5) Uani 1 1 d . . .
H12C H 0.4781 0.6557 0.9983 0.031 Uiso 1 1 calc R . .
C13C C 0.6067(2) 0.7806(2) 1.07966(19) 0.0382(7) Uani 1 1 d . . .
H13D H 0.6664 0.7494 1.0934 0.046 Uiso 1 1 calc R . .
C14C C 0.6323(3) 0.8803(2) 1.11680(19) 0.0410(7) Uani 1 1 d . . .
H14D H 0.7097 0.9184 1.1554 0.049 Uiso 1 1 calc R . .
C15C C 0.5434(2) 0.92433(19) 1.09702(19) 0.0363(6) Uani 1 1 d . . .
H15D H 0.5587 0.9934 1.1235 0.044 Uiso 1 1 calc R . .
C16C C 0.4323(2) 0.86835(17) 1.03883(17) 0.0274(5) Uani 1 1 d . . .
H16C H 0.3728 0.9004 1.0262 0.033 Uiso 1 1 calc R . .
C21C C 0.2776(2) 0.71818(15) 0.82572(16) 0.0203(5) Uani 1 1 d . . .
C22C C 0.3685(2) 0.78785(17) 0.80966(18) 0.0258(5) Uani 1 1 d . . .
H22C H 0.4285 0.8343 0.8612 0.031 Uiso 1 1 calc R . .
C23C C 0.3746(3) 0.7920(2) 0.7209(2) 0.0379(7) Uani 1 1 d . . .
H23C H 0.4392 0.8397 0.7128 0.045 Uiso 1 1 calc R . .
C24C C 0.2875(3) 0.7272(2) 0.6451(2) 0.0412(7) Uani 1 1 d . . .
H24C H 0.2919 0.7292 0.5844 0.049 Uiso 1 1 calc R . .
C25C C 0.1936(3) 0.65924(19) 0.65889(19) 0.0363(6) Uani 1 1 d . . .
H25C H 0.1313 0.6153 0.6078 0.044 Uiso 1 1 calc R . .
C26C C 0.1900(2) 0.65503(17) 0.74673(17) 0.0273(5) Uani 1 1 d . . .
H26C H 0.1250 0.6070 0.7540 0.033 Uiso 1 1 calc R . .
C31C C 0.1553(2) 0.74334(15) 0.98388(16) 0.0200(5) Uani 1 1 d . . .
C32C C 0.0548(2) 0.76582(17) 0.94538(18) 0.0262(5) Uani 1 1 d . . .
H32C H 0.0509 0.7566 0.8806 0.031 Uiso 1 1 calc R . .
C33C C -0.0400(2) 0.80134(18) 0.9993(2) 0.0342(6) Uani 1 1 d . . .
H33C H -0.1055 0.8175 0.9713 0.041 Uiso 1 1 calc R . .
C34C C -0.0396(2) 0.81311(17) 1.0926(2) 0.0325(6) Uani 1 1 d . . .
H34C H -0.1043 0.8372 1.1291 0.039 Uiso 1 1 calc R . .
C35C C 0.0561(2) 0.78933(16) 1.13218(18) 0.0281(6) Uani 1 1 d . . .
H35C H 0.0566 0.7954 1.1960 0.034 Uiso 1 1 calc R . .
C36C C 0.1517(2) 0.75662(16) 1.07899(17) 0.0237(5) Uani 1 1 d . . .
H36C H 0.2179 0.7425 1.1085 0.028 Uiso 1 1 calc R . .
C41C C 0.2534(2) 0.58690(16) 0.89922(16) 0.0198(5) Uani 1 1 d . . .
C42C C 0.1633(2) 0.53274(17) 0.93342(18) 0.0271(5) Uani 1 1 d . . .
H42C H 0.1089 0.5651 0.9759 0.032 Uiso 1 1 calc R . .
C43C C 0.1494(3) 0.43354(18) 0.9082(2) 0.0351(6) Uani 1 1 d . . .
H43C H 0.0859 0.3996 0.9328 0.042 Uiso 1 1 calc R . .
C44C C 0.2274(3) 0.38441(18) 0.84739(19) 0.0340(6) Uani 1 1 d . . .
H44C H 0.2178 0.3165 0.8294 0.041 Uiso 1 1 calc R . .
C45C C 0.3200(2) 0.43548(18) 0.81303(18) 0.0308(6) Uani 1 1 d . . .
H45C H 0.3759 0.4031 0.7723 0.037 Uiso 1 1 calc R . .
C46C C 0.3309(2) 0.53401(17) 0.83818(17) 0.0261(5) Uani 1 1 d . . .
H46C H 0.3941 0.5673 0.8128 0.031 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Rh1 0.02265(11) 0.01693(10) 0.01974(11) 0.00793(8) 0.00552(7) 0.00327(7)
N1 0.0212(10) 0.0179(10) 0.0219(10) 0.0078(8) 0.0059(8) 0.0053(8)
C2 0.0198(11) 0.0228(12) 0.0239(13) 0.0125(10) 0.0064(10) 0.0051(10)
N3 0.0251(10) 0.0217(10) 0.0248(11) 0.0101(9) 0.0108(9) 0.0064(8)
C4 0.0305(13) 0.0279(13) 0.0237(13) 0.0077(11) 0.0110(11) 0.0120(11)
C5 0.0284(13) 0.0215(12) 0.0258(13) 0.0055(11) 0.0077(11) 0.0077(11)
N1' 0.0305(11) 0.0316(11) 0.0330(12) 0.0206(10) 0.0032(10) 0.0050(10)
N2' 0.0245(10) 0.0285(11) 0.0325(12) 0.0171(10) 0.0050(9) 0.0059(9)
N3' 0.0210(10) 0.0222(10) 0.0279(11) 0.0130(9) 0.0064(9) 0.0037(8)
C4' 0.0248(12) 0.0228(12) 0.0264(13) 0.0118(11) 0.0073(10) 0.0012(10)
C5' 0.0324(14) 0.0343(14) 0.0294(14) 0.0175(12) 0.0074(11) 0.0056(12)
C6 0.0229(12) 0.0128(10) 0.0177(12) 0.0035(9) 0.0036(9) 0.0007(9)
C7 0.0244(12) 0.0194(12) 0.0202(12) 0.0051(10) 0.0018(10) 0.0041(10)
C8 0.0215(12) 0.0289(13) 0.0216(13) 0.0046(11) 0.0025(10) 0.0006(10)
C9 0.0335(14) 0.0300(14) 0.0193(13) 0.0090(11) 0.0012(11) -0.0077(11)
C10 0.0403(15) 0.0237(13) 0.0263(14) 0.0151(11) -0.0030(11) -0.0008(11)
C11 0.0284(13) 0.0181(11) 0.0226(13) 0.0057(10) -0.0020(10) 0.0030(10)
C12 0.0278(13) 0.0353(14) 0.0414(16) 0.0198(13) 0.0061(12) 0.0135(12)
C13 0.0434(17) 0.060(2) 0.0385(17) 0.0273(16) 0.0018(14) -0.0144(15)
C14 0.0335(14) 0.0318(14) 0.0435(17) 0.0185(13) -0.0011(12) 0.0106(12)
C6' 0.0358(15) 0.0445(16) 0.0513(18) 0.0347(15) 0.0054(13) 0.0147(13)
C7' 0.0337(14) 0.0366(15) 0.0403(16) 0.0299(13) 0.0108(12) 0.0166(12)
C8' 0.067(2) 0.0439(18) 0.062(2) 0.0339(18) 0.0333(18) 0.0159(17)
C9' 0.102(3) 0.0424(19) 0.044(2) 0.0207(17) 0.021(2) 0.024(2)
C10' 0.060(2) 0.0423(18) 0.069(2) 0.0311(18) -0.0001(18) 0.0078(16)
C11' 0.0389(17) 0.052(2) 0.075(3) 0.0338(19) 0.0149(17) 0.0089(15)
C12' 0.0386(16) 0.0505(18) 0.0461(18) 0.0285(16) 0.0138(14) 0.0164(14)
C1A 0.0277(13) 0.0272(13) 0.0359(15) 0.0171(12) 0.0159(11) 0.0053(11)
C1B 0.0373(14) 0.0278(13) 0.0219(13) 0.0122(11) 0.0044(11) 0.0112(11)
C2B 0.0373(14) 0.0205(12) 0.0174(12) 0.0072(10) 0.0006(11) 0.0002(11)
C3B 0.0362(14) 0.0296(14) 0.0238(13) 0.0117(11) 0.0066(11) 0.0008(11)
C4B 0.0318(14) 0.0307(14) 0.0283(14) 0.0097(12) 0.0117(11) 0.0065(11)
C5B 0.0314(13) 0.0210(12) 0.0233(13) 0.0065(11) 0.0057(11) 0.0061(11)
C6B 0.0344(14) 0.0191(12) 0.0227(13) 0.0049(10) 0.0074(11) 0.0026(11)
C7B 0.0333(14) 0.0289(14) 0.0280(14) 0.0075(12) -0.0014(11) -0.0044(11)
C8B 0.0315(14) 0.0397(15) 0.0358(16) 0.0175(13) -0.0013(12) 0.0050(12)
B1C 0.0185(13) 0.0187(13) 0.0199(14) 0.0082(11) 0.0011(11) 0.0040(10)
C11C 0.0170(11) 0.0245(12) 0.0181(12) 0.0094(10) 0.0072(9) 0.0053(10)
C12C 0.0244(12) 0.0313(13) 0.0244(13) 0.0134(11) 0.0038(10) 0.0068(11)
C13C 0.0252(14) 0.0566(19) 0.0344(16) 0.0210(15) -0.0041(12) 0.0089(13)
C14C 0.0262(14) 0.0528(19) 0.0280(15) 0.0074(14) -0.0044(12) -0.0051(13)
C15C 0.0337(15) 0.0282(14) 0.0309(15) 0.0015(12) 0.0065(12) -0.0049(12)
C16C 0.0238(12) 0.0266(13) 0.0281(14) 0.0078(11) 0.0039(11) 0.0052(11)
C21C 0.0223(12) 0.0179(11) 0.0232(12) 0.0083(10) 0.0049(10) 0.0100(10)
C22C 0.0242(12) 0.0283(13) 0.0305(14) 0.0160(11) 0.0055(11) 0.0092(11)
C23C 0.0403(16) 0.0446(16) 0.0459(18) 0.0321(15) 0.0178(14) 0.0171(14)
C24C 0.066(2) 0.0488(17) 0.0256(15) 0.0220(14) 0.0173(14) 0.0333(16)
C25C 0.0559(18) 0.0288(14) 0.0245(14) 0.0076(12) -0.0035(13) 0.0181(13)
C26C 0.0351(14) 0.0217(12) 0.0246(13) 0.0080(11) 0.0003(11) 0.0087(11)
C31C 0.0185(11) 0.0127(11) 0.0267(13) 0.0077(10) 0.0012(10) 0.0001(9)
C32C 0.0230(12) 0.0233(12) 0.0316(14) 0.0108(11) -0.0005(11) 0.0051(10)
C33C 0.0188(12) 0.0263(13) 0.0554(19) 0.0135(13) -0.0018(12) 0.0077(11)
C34C 0.0220(13) 0.0198(12) 0.0458(17) 0.0042(12) 0.0114(12) 0.0026(10)
C35C 0.0299(13) 0.0189(12) 0.0294(14) 0.0061(11) 0.0103(11) 0.0005(10)
C36C 0.0225(12) 0.0202(12) 0.0268(13) 0.0082(10) 0.0033(10) 0.0045(10)
C41C 0.0187(11) 0.0214(12) 0.0185(12) 0.0082(10) -0.0018(9) 0.0033(9)
C42C 0.0262(13) 0.0242(12) 0.0336(14) 0.0145(11) 0.0070(11) 0.0060(10)
C43C 0.0363(15) 0.0243(13) 0.0485(17) 0.0203(13) 0.0104(13) 0.0036(12)
C44C 0.0460(16) 0.0181(12) 0.0395(16) 0.0133(12) 0.0007(13) 0.0083(12)
C45C 0.0393(15) 0.0268(13) 0.0285(14) 0.0093(12) 0.0065(12) 0.0160(12)
C46C 0.0274(13) 0.0236(12) 0.0284(14) 0.0117(11) 0.0058(11) 0.0058(10)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 C2 2.047(2) . ?
Rh1 N3' 2.0848(18) . ?
Rh1 C1B 2.134(2) . ?
Rh1 C2B 2.154(2) . ?
Rh1 C5B 2.179(2) . ?
Rh1 C6B 2.202(2) . ?
N1 C2 1.359(3) . ?
N1 C5 1.387(3) . ?
N1 C6 1.441(3) . ?
C2 N3 1.357(3) . ?
N3 C4 1.378(3) . ?
N3 C1A 1.468(3) . ?
C4 C5 1.335(3) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
N1' N2' 1.339(3) . ?
N1' C5' 1.345(3) . ?
N1' C6' 1.472(3) . ?
N2' N3' 1.319(3) . ?
N3' C4' 1.357(3) . ?
C4' C5' 1.365(3) . ?
C4' C1A 1.488(3) . ?
C5' H5' 0.9500 . ?
C6 C11 1.390(3) . ?
C6 C7 1.398(3) . ?
C7 C8 1.385(3) . ?
C7 C12 1.498(3) . ?
C8 C9 1.392(3) . ?
C8 H9 0.9500 . ?
C9 C10 1.382(4) . ?
C9 C13 1.508(3) . ?
C10 C11 1.390(3) . ?
C10 H11 0.9500 . ?
C11 C14 1.505(3) . ?
C12 H13A 0.9800 . ?
C12 H13B 0.9800 . ?
C12 H13C 0.9800 . ?
C13 H14A 0.9800 . ?
C13 H14B 0.9800 . ?
C13 H14C 0.9800 . ?
C14 H15A 0.9800 . ?
C14 H15B 0.9800 . ?
C14 H15C 0.9800 . ?
C6' C7' 1.503(4) . ?
C6' H16A 0.9900 . ?
C6' H16B 0.9900 . ?
C7' C12' 1.379(4) . ?
C7' C8' 1.382(4) . ?
C8' C9' 1.391(5) . ?
C8' H22 0.9500 . ?
C9' C10' 1.370(5) . ?
C9' H9' 0.9500 . ?
C10' C11' 1.359(5) . ?
C10' H10' 0.9500 . ?
C11' C12' 1.380(4) . ?
C11' H11' 0.9500 . ?
C12' H18 0.9500 . ?
C1A H1A 0.9900 . ?
C1A H1B 0.9900 . ?
C1B C2B 1.386(3) . ?
C1B C8B 1.506(4) . ?
C1B H1B1 0.9500 . ?
C2B C3B 1.515(3) . ?
C2B H2B 0.9500 . ?
C3B C4B 1.534(3) . ?
C3B H3B1 0.9900 . ?
C3B H3B2 0.9900 . ?
C4B C5B 1.508(3) . ?
C4B H4B1 0.9900 . ?
C4B H4B2 0.9900 . ?
C5B C6B 1.375(3) . ?
C5B H5B 0.9500 . ?
C6B C7B 1.509(4) . ?
C6B H6B 0.9500 . ?
C7B C8B 1.534(4) . ?
C7B H7B1 0.9900 . ?
C7B H7B2 0.9900 . ?
C8B H8B1 0.9900 . ?
C8B H8B2 0.9900 . ?
B1C C31C 1.633(3) . ?
B1C C11C 1.642(3) . ?
B1C C41C 1.646(3) . ?
B1C C21C 1.651(3) . ?
C11C C12C 1.394(3) . ?
C11C C16C 1.408(3) . ?
C12C C13C 1.393(4) . ?
C12C H12C 0.9500 . ?
C13C C14C 1.370(4) . ?
C13C H13D 0.9500 . ?
C14C C15C 1.381(4) . ?
C14C H14D 0.9500 . ?
C15C C16C 1.383(4) . ?
C15C H15D 0.9500 . ?
C16C H16C 0.9500 . ?
C21C C22C 1.396(3) . ?
C21C C26C 1.402(3) . ?
C22C C23C 1.395(4) . ?
C22C H22C 0.9500 . ?
C23C C24C 1.378(4) . ?
C23C H23C 0.9500 . ?
C24C C25C 1.380(4) . ?
C24C H24C 0.9500 . ?
C25C C26C 1.381(3) . ?
C25C H25C 0.9500 . ?
C26C H26C 0.9500 . ?
C31C C32C 1.399(3) . ?
C31C C36C 1.400(3) . ?
C32C C33C 1.397(3) . ?
C32C H32C 0.9500 . ?
C33C C34C 1.375(4) . ?
C33C H33C 0.9500 . ?
C34C C35C 1.378(4) . ?
C34C H34C 0.9500 . ?
C35C C36C 1.385(3) . ?
C35C H35C 0.9500 . ?
C36C H36C 0.9500 . ?
C41C C42C 1.394(3) . ?
C41C C46C 1.401(3) . ?
C42C C43C 1.391(3) . ?
C42C H42C 0.9500 . ?
C43C C44C 1.379(4) . ?
C43C H43C 0.9500 . ?
C44C C45C 1.384(4) . ?
C44C H44C 0.9500 . ?
C45C C46C 1.385(3) . ?
C45C H45C 0.9500 . ?
C46C H46C 0.9500 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Rh1 N3' 85.57(8) . . ?
C2 Rh1 C1B 92.65(9) . . ?
N3' Rh1 C1B 151.19(9) . . ?
C2 Rh1 C2B 98.21(9) . . ?
N3' Rh1 C2B 170.59(8) . . ?
C1B Rh1 C2B 37.71(9) . . ?
C2 Rh1 C5B 162.30(9) . . ?
N3' Rh1 C5B 92.38(8) . . ?
C1B Rh1 C5B 97.44(9) . . ?
C2B Rh1 C5B 81.39(9) . . ?
C2 Rh1 C6B 160.70(9) . . ?
N3' Rh1 C6B 90.64(8) . . ?
C1B Rh1 C6B 81.62(9) . . ?
C2B Rh1 C6B 88.53(9) . . ?
C5B Rh1 C6B 36.58(9) . . ?
C2 N1 C5 111.39(18) . . ?
C2 N1 C6 125.44(18) . . ?
C5 N1 C6 122.67(18) . . ?
N3 C2 N1 103.21(19) . . ?
N3 C2 Rh1 121.73(15) . . ?
N1 C2 Rh1 134.90(16) . . ?
C2 N3 C4 112.02(19) . . ?
C2 N3 C1A 122.88(19) . . ?
C4 N3 C1A 125.09(19) . . ?
C5 C4 N3 106.6(2) . . ?
C5 C4 H4 126.7 . . ?
N3 C4 H4 126.7 . . ?
C4 C5 N1 106.7(2) . . ?
C4 C5 H5 126.6 . . ?
N1 C5 H5 126.6 . . ?
N2' N1' C5' 111.83(19) . . ?
N2' N1' C6' 119.0(2) . . ?
C5' N1' C6' 128.8(2) . . ?
N3' N2' N1' 105.60(18) . . ?
N2' N3' C4' 110.23(18) . . ?
N2' N3' Rh1 127.29(15) . . ?
C4' N3' Rh1 122.26(15) . . ?
N3' C4' C5' 107.4(2) . . ?
N3' C4' C1A 120.9(2) . . ?
C5' C4' C1A 131.6(2) . . ?
N1' C5' C4' 104.9(2) . . ?
N1' C5' H5' 127.5 . . ?
C4' C5' H5' 127.5 . . ?
C11 C6 C7 122.6(2) . . ?
C11 C6 N1 119.45(19) . . ?
C7 C6 N1 117.87(19) . . ?
C8 C7 C6 117.2(2) . . ?
C8 C7 C12 121.4(2) . . ?
C6 C7 C12 121.3(2) . . ?
C7 C8 C9 122.3(2) . . ?
C7 C8 H9 118.9 . . ?
C9 C8 H9 118.9 . . ?
C10 C9 C8 118.0(2) . . ?
C10 C9 C13 121.5(2) . . ?
C8 C9 C13 120.4(2) . . ?
C9 C10 C11 122.4(2) . . ?
C9 C10 H11 118.8 . . ?
C11 C10 H11 118.8 . . ?
C6 C11 C10 117.3(2) . . ?
C6 C11 C14 121.5(2) . . ?
C10 C11 C14 121.1(2) . . ?
C7 C12 H13A 109.5 . . ?
C7 C12 H13B 109.5 . . ?
H13A C12 H13B 109.5 . . ?
C7 C12 H13C 109.5 . . ?
H13A C12 H13C 109.5 . . ?
H13B C12 H13C 109.5 . . ?
C9 C13 H14A 109.5 . . ?
C9 C13 H14B 109.5 . . ?
H14A C13 H14B 109.5 . . ?
C9 C13 H14C 109.5 . . ?
H14A C13 H14C 109.5 . . ?
H14B C13 H14C 109.5 . . ?
C11 C14 H15A 109.5 . . ?
C11 C14 H15B 109.5 . . ?
H15A C14 H15B 109.5 . . ?
C11 C14 H15C 109.5 . . ?
H15A C14 H15C 109.5 . . ?
H15B C14 H15C 109.5 . . ?
N1' C6' C7' 110.6(2) . . ?
N1' C6' H16A 109.5 . . ?
C7' C6' H16A 109.5 . . ?
N1' C6' H16B 109.5 . . ?
C7' C6' H16B 109.5 . . ?
H16A C6' H16B 108.1 . . ?
C12' C7' C8' 117.9(3) . . ?
C12' C7' C6' 120.8(3) . . ?
C8' C7' C6' 121.3(2) . . ?
C7' C8' C9' 120.8(3) . . ?
C7' C8' H22 119.6 . . ?
C9' C8' H22 119.6 . . ?
C10' C9' C8' 119.9(3) . . ?
C10' C9' H9' 120.1 . . ?
C8' C9' H9' 120.1 . . ?
C11' C10' C9' 119.9(3) . . ?
C11' C10' H10' 120.0 . . ?
C9' C10' H10' 120.0 . . ?
C10' C11' C12' 120.3(3) . . ?
C10' C11' H11' 119.8 . . ?
C12' C11' H11' 119.8 . . ?
C7' C12' C11' 121.2(3) . . ?
C7' C12' H18 119.4 . . ?
C11' C12' H18 119.4 . . ?
N3 C1A C4' 110.94(18) . . ?
N3 C1A H1A 109.5 . . ?
C4' C1A H1A 109.5 . . ?
N3 C1A H1B 109.5 . . ?
C4' C1A H1B 109.5 . . ?
H1A C1A H1B 108.0 . . ?
C2B C1B C8B 125.9(2) . . ?
C2B C1B Rh1 71.94(14) . . ?
C8B C1B Rh1 108.82(15) . . ?
C2B C1B H1B1 117.0 . . ?
C8B C1B H1B1 117.0 . . ?
Rh1 C1B H1B1 89.2 . . ?
C1B C2B C3B 124.7(2) . . ?
C1B C2B Rh1 70.35(13) . . ?
C3B C2B Rh1 112.71(15) . . ?
C1B C2B H2B 117.7 . . ?
C3B C2B H2B 117.7 . . ?
Rh1 C2B H2B 86.9 . . ?
C2B C3B C4B 112.5(2) . . ?
C2B C3B H3B1 109.1 . . ?
C4B C3B H3B1 109.1 . . ?
C2B C3B H3B2 109.1 . . ?
C4B C3B H3B2 109.1 . . ?
H3B1 C3B H3B2 107.8 . . ?
C5B C4B C3B 112.9(2) . . ?
C5B C4B H4B1 109.0 . . ?
C3B C4B H4B1 109.0 . . ?
C5B C4B H4B2 109.0 . . ?
C3B C4B H4B2 109.0 . . ?
H4B1 C4B H4B2 107.8 . . ?
C6B C5B C4B 126.1(2) . . ?
C6B C5B Rh1 72.61(14) . . ?
C4B C5B Rh1 108.18(15) . . ?
C6B C5B H5B 116.9 . . ?
C4B C5B H5B 116.9 . . ?
Rh1 C5B H5B 89.2 . . ?
C5B C6B C7B 125.3(2) . . ?
C5B C6B Rh1 70.81(14) . . ?
C7B C6B Rh1 111.24(16) . . ?
C5B C6B H6B 117.3 . . ?
C7B C6B H6B 117.3 . . ?
Rh1 C6B H6B 87.9 . . ?
C6B C7B C8B 112.4(2) . . ?
C6B C7B H7B1 109.1 . . ?
C8B C7B H7B1 109.1 . . ?
C6B C7B H7B2 109.1 . . ?
C8B C7B H7B2 109.1 . . ?
H7B1 C7B H7B2 107.9 . . ?
C1B C8B C7B 113.7(2) . . ?
C1B C8B H8B1 108.8 . . ?
C7B C8B H8B1 108.8 . . ?
C1B C8B H8B2 108.8 . . ?
C7B C8B H8B2 108.8 . . ?
H8B1 C8B H8B2 107.7 . . ?
C31C B1C C11C 106.89(18) . . ?
C31C B1C C41C 110.56(18) . . ?
C11C B1C C41C 109.94(17) . . ?
C31C B1C C21C 112.03(17) . . ?
C11C B1C C21C 110.61(18) . . ?
C41C B1C C21C 106.84(18) . . ?
C12C C11C C16C 114.9(2) . . ?
C12C C11C B1C 125.0(2) . . ?
C16C C11C B1C 120.17(19) . . ?
C13C C12C C11C 122.5(2) . . ?
C13C C12C H12C 118.7 . . ?
C11C C12C H12C 118.7 . . ?
C14C C13C C12C 120.7(2) . . ?
C14C C13C H13D 119.7 . . ?
C12C C13C H13D 119.7 . . ?
C13C C14C C15C 118.8(2) . . ?
C13C C14C H14D 120.6 . . ?
C15C C14C H14D 120.6 . . ?
C14C C15C C16C 120.3(2) . . ?
C14C C15C H15D 119.9 . . ?
C16C C15C H15D 119.9 . . ?
C15C C16C C11C 122.8(2) . . ?
C15C C16C H16C 118.6 . . ?
C11C C16C H16C 118.6 . . ?
C22C C21C C26C 114.8(2) . . ?
C22C C21C B1C 125.0(2) . . ?
C26C C21C B1C 120.1(2) . . ?
C23C C22C C21C 122.6(2) . . ?
C23C C22C H22C 118.7 . . ?
C21C C22C H22C 118.7 . . ?
C24C C23C C22C 120.3(2) . . ?
C24C C23C H23C 119.9 . . ?
C22C C23C H23C 119.9 . . ?
C23C C24C C25C 118.9(2) . . ?
C23C C24C H24C 120.6 . . ?
C25C C24C H24C 120.6 . . ?
C24C C25C C26C 120.1(3) . . ?
C24C C25C H25C 119.9 . . ?
C26C C25C H25C 119.9 . . ?
C25C C26C C21C 123.2(2) . . ?
C25C C26C H26C 118.4 . . ?
C21C C26C H26C 118.4 . . ?
C32C C31C C36C 115.1(2) . . ?
C32C C31C B1C 125.1(2) . . ?
C36C C31C B1C 119.80(19) . . ?
C33C C32C C31C 122.0(2) . . ?
C33C C32C H32C 119.0 . . ?
C31C C32C H32C 119.0 . . ?
C34C C33C C32C 120.8(2) . . ?
C34C C33C H33C 119.6 . . ?
C32C C33C H33C 119.6 . . ?
C33C C34C C35C 118.8(2) . . ?
C33C C34C H34C 120.6 . . ?
C35C C34C H34C 120.6 . . ?
C34C C35C C36C 120.1(2) . . ?
C34C C35C H35C 120.0 . . ?
C36C C35C H35C 120.0 . . ?
C35C C36C C31C 123.2(2) . . ?
C35C C36C H36C 118.4 . . ?
C31C C36C H36C 118.4 . . ?
C42C C41C C46C 114.8(2) . . ?
C42C C41C B1C 124.4(2) . . ?
C46C C41C B1C 120.80(19) . . ?
C43C C42C C41C 123.0(2) . . ?
C43C C42C H42C 118.5 . . ?
C41C C42C H42C 118.5 . . ?
C44C C43C C42C 120.1(2) . . ?
C44C C43C H43C 119.9 . . ?
C42C C43C H43C 119.9 . . ?
C43C C44C C45C 119.0(2) . . ?
C43C C44C H44C 120.5 . . ?
C45C C44C H44C 120.5 . . ?
C44C C45C C46C 119.8(2) . . ?
C44C C45C H45C 120.1 . . ?
C46C C45C H45C 120.1 . . ?
C45C C46C C41C 123.2(2) . . ?
C45C C46C H46C 118.4 . . ?
C41C C46C H46C 118.4 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 C2 N3 0.3(2) . . . . ?
C6 N1 C2 N3 172.36(19) . . . . ?
C5 N1 C2 Rh1 -174.95(18) . . . . ?
C6 N1 C2 Rh1 -2.9(4) . . . . ?
N3' Rh1 C2 N3 -35.62(18) . . . . ?
C1B Rh1 C2 N3 115.57(19) . . . . ?
C2B Rh1 C2 N3 153.06(18) . . . . ?
C5B Rh1 C2 N3 -119.6(3) . . . . ?
C6B Rh1 C2 N3 43.6(4) . . . . ?
N3' Rh1 C2 N1 138.9(2) . . . . ?
C1B Rh1 C2 N1 -69.9(2) . . . . ?
C2B Rh1 C2 N1 -32.4(2) . . . . ?
C5B Rh1 C2 N1 55.0(4) . . . . ?
C6B Rh1 C2 N1 -141.9(3) . . . . ?
N1 C2 N3 C4 0.0(2) . . . . ?
Rh1 C2 N3 C4 176.02(16) . . . . ?
N1 C2 N3 C1A -178.9(2) . . . . ?
Rh1 C2 N3 C1A -2.9(3) . . . . ?
C2 N3 C4 C5 -0.3(3) . . . . ?
C1A N3 C4 C5 178.6(2) . . . . ?
N3 C4 C5 N1 0.4(3) . . . . ?
C2 N1 C5 C4 -0.5(3) . . . . ?
C6 N1 C5 C4 -172.8(2) . . . . ?
C5' N1' N2' N3' 0.1(3) . . . . ?
C6' N1' N2' N3' 173.5(2) . . . . ?
N1' N2' N3' C4' -0.1(3) . . . . ?
N1' N2' N3' Rh1 -174.69(15) . . . . ?
C2 Rh1 N3' N2' -147.6(2) . . . . ?
C1B Rh1 N3' N2' 125.0(2) . . . . ?
C2B Rh1 N3' N2' -33.5(6) . . . . ?
C5B Rh1 N3' N2' 14.8(2) . . . . ?
C6B Rh1 N3' N2' 51.37(19) . . . . ?
C2 Rh1 N3' C4' 38.39(19) . . . . ?
C1B Rh1 N3' C4' -49.1(3) . . . . ?
C2B Rh1 N3' C4' 152.5(5) . . . . ?
C5B Rh1 N3' C4' -159.22(19) . . . . ?
C6B Rh1 N3' C4' -122.67(19) . . . . ?
N2' N3' C4' C5' 0.0(3) . . . . ?
Rh1 N3' C4' C5' 174.94(16) . . . . ?
N2' N3' C4' C1A -177.4(2) . . . . ?
Rh1 N3' C4' C1A -2.5(3) . . . . ?
N2' N1' C5' C4' -0.1(3) . . . . ?
C6' N1' C5' C4' -172.6(2) . . . . ?
N3' C4' C5' N1' 0.1(3) . . . . ?
C1A C4' C5' N1' 177.1(3) . . . . ?
C2 N1 C6 C11 110.6(2) . . . . ?
C5 N1 C6 C11 -78.2(3) . . . . ?
C2 N1 C6 C7 -71.4(3) . . . . ?
C5 N1 C6 C7 99.8(2) . . . . ?
C11 C6 C7 C8 -0.8(3) . . . . ?
N1 C6 C7 C8 -178.8(2) . . . . ?
C11 C6 C7 C12 177.5(2) . . . . ?
N1 C6 C7 C12 -0.4(3) . . . . ?
C6 C7 C8 C9 2.5(3) . . . . ?
C12 C7 C8 C9 -175.8(2) . . . . ?
C7 C8 C9 C10 -2.4(4) . . . . ?
C7 C8 C9 C13 174.5(2) . . . . ?
C8 C9 C10 C11 0.6(4) . . . . ?
C13 C9 C10 C11 -176.3(2) . . . . ?
C7 C6 C11 C10 -0.9(3) . . . . ?
N1 C6 C11 C10 177.1(2) . . . . ?
C7 C6 C11 C14 179.6(2) . . . . ?
N1 C6 C11 C14 -2.4(3) . . . . ?
C9 C10 C11 C6 1.0(4) . . . . ?
C9 C10 C11 C14 -179.5(2) . . . . ?
N2' N1' C6' C7' -82.4(3) . . . . ?
C5' N1' C6' C7' 89.6(3) . . . . ?
N1' C6' C7' C12' -89.6(3) . . . . ?
N1' C6' C7' C8' 88.1(3) . . . . ?
C12' C7' C8' C9' 0.3(4) . . . . ?
C6' C7' C8' C9' -177.5(3) . . . . ?
C7' C8' C9' C10' -0.1(5) . . . . ?
C8' C9' C10' C11' -0.7(5) . . . . ?
C9' C10' C11' C12' 1.2(5) . . . . ?
C8' C7' C12' C11' 0.2(4) . . . . ?
C6' C7' C12' C11' 178.1(2) . . . . ?
C10' C11' C12' C7' -1.0(4) . . . . ?
C2 N3 C1A C4' 53.6(3) . . . . ?
C4 N3 C1A C4' -125.1(2) . . . . ?
N3' C4' C1A N3 -49.7(3) . . . . ?
C5' C4' C1A N3 133.6(3) . . . . ?
C2 Rh1 C1B C2B 100.00(15) . . . . ?
N3' Rh1 C1B C2B -174.37(15) . . . . ?
C5B Rh1 C1B C2B -65.43(15) . . . . ?
C6B Rh1 C1B C2B -98.52(15) . . . . ?
C2 Rh1 C1B C8B -137.27(17) . . . . ?
N3' Rh1 C1B C8B -51.6(3) . . . . ?
C2B Rh1 C1B C8B 122.7(2) . . . . ?
C5B Rh1 C1B C8B 57.30(18) . . . . ?
C6B Rh1 C1B C8B 24.21(17) . . . . ?
C8B C1B C2B C3B 4.0(4) . . . . ?
Rh1 C1B C2B C3B 104.6(2) . . . . ?
C8B C1B C2B Rh1 -100.5(2) . . . . ?
C2 Rh1 C2B C1B -83.68(15) . . . . ?
N3' Rh1 C2B C1B 163.2(5) . . . . ?
C5B Rh1 C2B C1B 114.20(15) . . . . ?
C6B Rh1 C2B C1B 78.16(15) . . . . ?
C2 Rh1 C2B C3B 155.98(18) . . . . ?
N3' Rh1 C2B C3B 42.8(6) . . . . ?
C1B Rh1 C2B C3B -120.3(2) . . . . ?
C5B Rh1 C2B C3B -6.13(18) . . . . ?
C6B Rh1 C2B C3B -42.18(18) . . . . ?
C1B C2B C3B C4B -94.2(3) . . . . ?
Rh1 C2B C3B C4B -13.0(3) . . . . ?
C2B C3B C4B C5B 34.7(3) . . . . ?
C3B C4B C5B C6B 43.0(3) . . . . ?
C3B C4B C5B Rh1 -38.4(3) . . . . ?
C2 Rh1 C5B C6B 170.7(2) . . . . ?
N3' Rh1 C5B C6B 87.86(14) . . . . ?
C1B Rh1 C5B C6B -65.00(15) . . . . ?
C2B Rh1 C5B C6B -99.23(15) . . . . ?
C2 Rh1 C5B C4B -66.1(3) . . . . ?
N3' Rh1 C5B C4B -148.97(17) . . . . ?
C1B Rh1 C5B C4B 58.18(18) . . . . ?
C2B Rh1 C5B C4B 23.94(17) . . . . ?
C6B Rh1 C5B C4B 123.2(2) . . . . ?
C4B C5B C6B C7B 2.8(4) . . . . ?
Rh1 C5B C6B C7B 102.9(2) . . . . ?
C4B C5B C6B Rh1 -100.2(2) . . . . ?
C2 Rh1 C6B C5B -171.5(2) . . . . ?
N3' Rh1 C6B C5B -93.14(14) . . . . ?
C1B Rh1 C6B C5B 114.72(15) . . . . ?
C2B Rh1 C6B C5B 77.48(15) . . . . ?
C2 Rh1 C6B C7B 67.1(3) . . . . ?
N3' Rh1 C6B C7B 145.43(17) . . . . ?
C1B Rh1 C6B C7B -6.70(17) . . . . ?
C2B Rh1 C6B C7B -43.94(18) . . . . ?
C5B Rh1 C6B C7B -121.4(2) . . . . ?
C5B C6B C7B C8B -93.2(3) . . . . ?
Rh1 C6B C7B C8B -12.2(3) . . . . ?
C2B C1B C8B C7B 42.1(3) . . . . ?
Rh1 C1B C8B C7B -38.9(3) . . . . ?
C6B C7B C8B C1B 34.2(3) . . . . ?
C31C B1C C11C C12C 127.1(2) . . . . ?
C41C B1C C11C C12C 7.0(3) . . . . ?
C21C B1C C11C C12C -110.7(2) . . . . ?
C31C B1C C11C C16C -53.0(3) . . . . ?
C41C B1C C11C C16C -173.08(19) . . . . ?
C21C B1C C11C C16C 69.2(3) . . . . ?
C16C C11C C12C C13C -2.5(3) . . . . ?
B1C C11C C12C C13C 177.4(2) . . . . ?
C11C C12C C13C C14C 1.3(4) . . . . ?
C12C C13C C14C C15C 0.9(4) . . . . ?
C13C C14C C15C C16C -1.6(4) . . . . ?
C14C C15C C16C C11C 0.2(4) . . . . ?
C12C C11C C16C C15C 1.8(3) . . . . ?
B1C C11C C16C C15C -178.1(2) . . . . ?
C31C B1C C21C C22C 106.6(2) . . . . ?
C11C B1C C21C C22C -12.6(3) . . . . ?
C41C B1C C21C C22C -132.2(2) . . . . ?
C31C B1C C21C C26C -76.0(3) . . . . ?
C11C B1C C21C C26C 164.87(19) . . . . ?
C41C B1C C21C C26C 45.2(3) . . . . ?
C26C C21C C22C C23C -2.3(3) . . . . ?
B1C C21C C22C C23C 175.2(2) . . . . ?
C21C C22C C23C C24C 1.4(4) . . . . ?
C22C C23C C24C C25C 0.8(4) . . . . ?
C23C C24C C25C C26C -1.8(4) . . . . ?
C24C C25C C26C C21C 0.8(4) . . . . ?
C22C C21C C26C C25C 1.3(3) . . . . ?
B1C C21C C26C C25C -176.4(2) . . . . ?
C11C B1C C31C C32C 135.0(2) . . . . ?
C41C B1C C31C C32C -105.3(2) . . . . ?
C21C B1C C31C C32C 13.7(3) . . . . ?
C11C B1C C31C C36C -45.1(3) . . . . ?
C41C B1C C31C C36C 74.6(3) . . . . ?
C21C B1C C31C C36C -166.36(19) . . . . ?
C36C C31C C32C C33C 1.6(3) . . . . ?
B1C C31C C32C C33C -178.5(2) . . . . ?
C31C C32C C33C C34C -1.8(4) . . . . ?
C32C C33C C34C C35C 0.1(4) . . . . ?
C33C C34C C35C C36C 1.7(4) . . . . ?
C34C C35C C36C C31C -1.8(4) . . . . ?
C32C C31C C36C C35C 0.1(3) . . . . ?
B1C C31C C36C C35C -179.8(2) . . . . ?
C31C B1C C41C C42C -9.6(3) . . . . ?
C11C B1C C41C C42C 108.2(2) . . . . ?
C21C B1C C41C C42C -131.7(2) . . . . ?
C31C B1C C41C C46C 170.7(2) . . . . ?
C11C B1C C41C C46C -71.5(3) . . . . ?
C21C B1C C41C C46C 48.5(3) . . . . ?
C46C C41C C42C C43C -1.0(4) . . . . ?
B1C C41C C42C C43C 179.3(2) . . . . ?
C41C C42C C43C C44C 0.6(4) . . . . ?
C42C C43C C44C C45C 0.6(4) . . . . ?
C43C C44C C45C C46C -1.5(4) . . . . ?
C44C C45C C46C C41C 1.2(4) . . . . ?
C42C C41C C46C C45C 0.1(3) . . . . ?
B1C C41C C46C C45C 179.8(2) . . . . ?
_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max 1.132
_refine_diff_density_min -0.398
_refine_diff_density_rms 0.058
_database_code_depnum_ccdc_archive 'CCDC 934035'
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_khuong3_pbca
#TrackingRef 'Khuong3_Deposition_15May12.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C24 H23 N5 O2 Rh, C24 H20 B'
_chemical_formula_sum 'C48 H43 B N5 O2 Rh'
_chemical_formula_weight 835.59
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Orthorhombic
_symmetry_space_group_name_H-M Pbca
_symmetry_space_group_name_Hall '-P 2ac 2ab'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
_cell_length_a 15.4027(11)
_cell_length_b 16.4453(15)
_cell_length_c 33.125(3)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 8390.7(12)
_cell_formula_units_Z 8
_cell_measurement_temperature 150(2)
_cell_measurement_reflns_used 982
_cell_measurement_theta_min 2.584
_cell_measurement_theta_max 16.486
_exptl_crystal_description Plates
_exptl_crystal_colour 'Red orange'
_exptl_crystal_size_max 0.28
_exptl_crystal_size_mid 0.09
_exptl_crystal_size_min 0.04
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.323
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 3456
_exptl_absorpt_coefficient_mu 0.452
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.8858
_exptl_absorpt_correction_T_max 0.9844
_exptl_absorpt_process_details 'SADABS (Bruker, 2001)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 150(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker kappa APEXII CCD Diffractometer'
_diffrn_measurement_method '\f scans, and \w scans with \k offsets'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 34660
_diffrn_reflns_av_R_equivalents 0.2098
_diffrn_reflns_av_sigmaI/netI 0.2437
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_l_min -28
_diffrn_reflns_limit_l_max 39
_diffrn_reflns_theta_min 1.81
_diffrn_reflns_theta_max 25.00
_reflns_number_total 7389
_reflns_number_gt 2965
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2007)'
_computing_cell_refinement 'APEX2 (Bruker, 2007)'
_computing_data_reduction 'APEX2 (Bruker, 2007)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
Crystals were thin plates (~ 0.04 mm thick) resulting in weak diffraction
(2965 observed of total of 7389 reflections) resulting in high Rint value
(0.21), which is an alert at level B.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0249P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 7389
_refine_ls_number_parameters 517
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.2041
_refine_ls_R_factor_gt 0.0606
_refine_ls_wR_factor_ref 0.1183
_refine_ls_wR_factor_gt 0.0824
_refine_ls_goodness_of_fit_ref 0.937
_refine_ls_restrained_S_all 0.937
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.53401(3) 0.40216(4) 1.007798(13) 0.02643(17) Uani 1 1 d . . .
N1 N 0.6913(3) 0.4313(4) 1.06545(15) 0.0245(16) Uani 1 1 d . . .
C2 C 0.6550(4) 0.4353(4) 1.02788(18) 0.0237(19) Uani 1 1 d . . .
N3 N 0.7196(3) 0.4676(3) 1.00557(15) 0.0261(14) Uani 1 1 d . . .
C4 C 0.7934(4) 0.4849(5) 1.0278(2) 0.035(2) Uani 1 1 d . . .
H4 H 0.8458 0.5086 1.0184 0.042 Uiso 1 1 calc R . .
C5 C 0.7750(4) 0.4609(5) 1.0657(2) 0.035(2) Uani 1 1 d . . .
H5 H 0.8127 0.4639 1.0883 0.042 Uiso 1 1 calc R . .
C1A C 0.7145(4) 0.4870(5) 0.96225(17) 0.028(2) Uani 1 1 d . . .
H1A1 H 0.7741 0.4916 0.9513 0.033 Uiso 1 1 calc R . .
H1A2 H 0.6858 0.5405 0.9589 0.033 Uiso 1 1 calc R . .
N1' N 0.6167(3) 0.3433(4) 0.89411(16) 0.0273(15) Uani 1 1 d . . .
N2' N 0.5581(3) 0.3429(4) 0.92359(16) 0.0251(15) Uani 1 1 d . . .
N3' N 0.5894(3) 0.3932(4) 0.95138(14) 0.0251(15) Uani 1 1 d . . .
C4' C 0.6661(4) 0.4251(5) 0.93880(19) 0.026(2) Uani 1 1 d . . .
C5' C 0.6842(4) 0.3927(5) 0.90225(19) 0.0299(19) Uani 1 1 d . . .
H5' H 0.7337 0.4027 0.8859 0.036 Uiso 1 1 calc R . .
C6 C 0.6512(4) 0.3947(6) 1.10087(19) 0.0276(19) Uani 1 1 d . . .
C7 C 0.6126(4) 0.4454(6) 1.1290(2) 0.036(2) Uani 1 1 d . . .
C8 C 0.5732(4) 0.4068(8) 1.1623(2) 0.057(3) Uani 1 1 d . . .
H8 H 0.5456 0.4397 1.1821 0.068 Uiso 1 1 calc R . .
C9 C 0.5727(5) 0.3235(8) 1.1674(3) 0.060(4) Uani 1 1 d . . .
C10 C 0.6152(5) 0.2773(6) 1.1389(3) 0.056(3) Uani 1 1 d . . .
H10 H 0.6166 0.2200 1.1423 0.067 Uiso 1 1 calc R . .
C11 C 0.6563(4) 0.3107(6) 1.1050(2) 0.036(2) Uani 1 1 d . . .
C12 C 0.6112(4) 0.5351(6) 1.1238(2) 0.061(3) Uani 1 1 d . . .
H12A H 0.6703 0.5565 1.1262 0.091 Uiso 1 1 calc R . .
H12B H 0.5745 0.5595 1.1447 0.091 Uiso 1 1 calc R . .
H12C H 0.5877 0.5485 1.0971 0.091 Uiso 1 1 calc R . .
C13 C 0.5268(5) 0.2853(7) 1.20258(19) 0.097(4) Uani 1 1 d . . .
H13A H 0.5097 0.3276 1.2218 0.145 Uiso 1 1 calc R . .
H13B H 0.5658 0.2466 1.2159 0.145 Uiso 1 1 calc R . .
H13C H 0.4750 0.2566 1.1930 0.145 Uiso 1 1 calc R . .
C14 C 0.7054(5) 0.2587(5) 1.0764(2) 0.061(3) Uani 1 1 d . . .
H14A H 0.6846 0.2684 1.0489 0.091 Uiso 1 1 calc R . .
H14B H 0.6969 0.2014 1.0835 0.091 Uiso 1 1 calc R . .
H14C H 0.7674 0.2720 1.0780 0.091 Uiso 1 1 calc R . .
C6' C 0.6040(4) 0.2931(5) 0.8578(2) 0.038(2) Uani 1 1 d . . .
H6'1 H 0.5667 0.2461 0.8648 0.045 Uiso 1 1 calc R . .
H6'2 H 0.6610 0.2715 0.8490 0.045 Uiso 1 1 calc R . .
C7' C 0.5627(5) 0.3389(5) 0.8227(2) 0.037(2) Uani 1 1 d . . .
C8' C 0.6058(5) 0.4035(6) 0.8053(2) 0.049(2) Uani 1 1 d . . .
H8' H 0.6614 0.4193 0.8150 0.059 Uiso 1 1 calc R . .
C9' C 0.5671(6) 0.4458(6) 0.7732(2) 0.060(3) Uani 1 1 d . . .
H9' H 0.5962 0.4908 0.7614 0.072 Uiso 1 1 calc R . .
C10' C 0.4874(6) 0.4226(6) 0.7589(2) 0.062(3) Uani 1 1 d . . .
H10' H 0.4617 0.4508 0.7369 0.074 Uiso 1 1 calc R . .
C11' C 0.4447(5) 0.3584(6) 0.7765(2) 0.055(3) Uani 1 1 d . . .
H11' H 0.3890 0.3429 0.7668 0.067 Uiso 1 1 calc R . .
C12' C 0.4824(5) 0.3159(5) 0.8083(2) 0.045(2) Uani 1 1 d . . .
H12' H 0.4529 0.2711 0.8200 0.054 Uiso 1 1 calc R . .
C1B C 0.4828(4) 0.4070(5) 1.05793(18) 0.0335(19) Uani 1 1 d . . .
O1B O 0.4422(2) 0.4112(4) 1.08711(12) 0.0438(16) Uani 1 1 d . . .
C2B C 0.4279(4) 0.3624(5) 0.9871(2) 0.034(2) Uani 1 1 d . . .
O2B O 0.3635(3) 0.3374(4) 0.97591(13) 0.0592(19) Uani 1 1 d . . .
B1D B 0.9233(5) 0.5354(6) 0.8723(2) 0.034(3) Uani 1 1 d . . .
C11D C 0.8544(4) 0.5764(5) 0.83948(19) 0.029(2) Uani 1 1 d . . .
C12D C 0.7647(4) 0.5722(4) 0.84717(19) 0.033(2) Uani 1 1 d . . .
H12D H 0.7457 0.5490 0.8719 0.040 Uiso 1 1 calc R . .
C13D C 0.7028(4) 0.6004(5) 0.8201(2) 0.0320(18) Uani 1 1 d . . .
H13D H 0.6428 0.5970 0.8267 0.038 Uiso 1 1 calc R . .
C14D C 0.7282(4) 0.6332(5) 0.78400(19) 0.039(2) Uani 1 1 d . . .
H14D H 0.6861 0.6525 0.7654 0.047 Uiso 1 1 calc R . .
C15D C 0.8159(4) 0.6380(5) 0.7748(2) 0.041(2) Uani 1 1 d . . .
H15D H 0.8343 0.6606 0.7498 0.050 Uiso 1 1 calc R . .
C16D C 0.8765(4) 0.6097(5) 0.8024(2) 0.039(2) Uani 1 1 d . . .
H16D H 0.9363 0.6132 0.7955 0.047 Uiso 1 1 calc R . .
C21D C 1.0235(4) 0.5407(6) 0.8545(2) 0.040(2) Uani 1 1 d . . .
C22D C 1.0677(4) 0.4731(7) 0.8401(2) 0.060(3) Uani 1 1 d . . .
H22D H 1.0402 0.4214 0.8414 0.072 Uiso 1 1 calc R . .
C23D C 1.1512(5) 0.4782(8) 0.8239(2) 0.078(4) Uani 1 1 d . . .
H23D H 1.1795 0.4307 0.8142 0.093 Uiso 1 1 calc R . .
C24D C 1.1917(6) 0.5512(9) 0.8221(3) 0.076(4) Uani 1 1 d . . .
H24D H 1.2477 0.5546 0.8101 0.091 Uiso 1 1 calc R . .
C25D C 1.1536(5) 0.6205(7) 0.8370(3) 0.080(4) Uani 1 1 d . . .
H25D H 1.1826 0.6714 0.8361 0.096 Uiso 1 1 calc R . .
C26D C 1.0696(5) 0.6132(6) 0.8539(2) 0.064(3) Uani 1 1 d . . .
H26D H 1.0435 0.6601 0.8654 0.077 Uiso 1 1 calc R . .
C31D C 0.9203(4) 0.5855(5) 0.91510(19) 0.033(2) Uani 1 1 d . . .
C32D C 0.9874(4) 0.5740(5) 0.9436(2) 0.042(2) Uani 1 1 d . . .
H32D H 1.0329 0.5371 0.9374 0.051 Uiso 1 1 calc R . .
C33D C 0.9895(4) 0.6138(5) 0.9799(2) 0.046(2) Uani 1 1 d . . .
H33D H 1.0365 0.6039 0.9977 0.055 Uiso 1 1 calc R . .
C34D C 0.9254(5) 0.6680(5) 0.9914(2) 0.045(2) Uani 1 1 d . . .
H34D H 0.9279 0.6958 1.0165 0.054 Uiso 1 1 calc R . .
C35D C 0.8574(4) 0.6798(5) 0.9646(2) 0.041(2) Uani 1 1 d . . .
H35D H 0.8112 0.7153 0.9717 0.049 Uiso 1 1 calc R . .
C36D C 0.8559(4) 0.6405(5) 0.9276(2) 0.033(2) Uani 1 1 d . . .
H36D H 0.8090 0.6513 0.9097 0.039 Uiso 1 1 calc R . .
C41D C 0.8978(4) 0.4405(5) 0.8779(2) 0.031(2) Uani 1 1 d . . .
C42D C 0.9071(4) 0.3972(6) 0.9136(2) 0.037(2) Uani 1 1 d . . .
H42D H 0.9279 0.4252 0.9367 0.044 Uiso 1 1 calc R . .
C43D C 0.8875(4) 0.3139(6) 0.9172(3) 0.052(3) Uani 1 1 d . . .
H43D H 0.8939 0.2870 0.9424 0.063 Uiso 1 1 calc R . .
C44D C 0.8585(4) 0.2716(5) 0.8833(3) 0.048(2) Uani 1 1 d . . .
H44D H 0.8450 0.2154 0.8850 0.057 Uiso 1 1 calc R . .
C45D C 0.8497(4) 0.3128(6) 0.8474(2) 0.043(2) Uani 1 1 d . . .
H45D H 0.8311 0.2844 0.8239 0.051 Uiso 1 1 calc R . .
C46D C 0.8678(4) 0.3953(6) 0.8449(2) 0.039(2) Uani 1 1 d . . .
H46D H 0.8596 0.4222 0.8198 0.047 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Rh1 0.0237(3) 0.0348(4) 0.0208(3) 0.0016(4) 0.0012(3) -0.0049(3)
N1 0.028(3) 0.027(5) 0.018(3) -0.001(3) -0.002(3) -0.001(3)
C2 0.017(4) 0.031(6) 0.023(4) 0.000(4) 0.003(3) 0.002(3)
N3 0.023(3) 0.038(4) 0.017(3) 0.004(3) 0.000(3) 0.002(3)
C4 0.016(4) 0.053(7) 0.036(5) 0.003(5) 0.001(3) -0.001(4)
C5 0.021(4) 0.047(7) 0.036(5) 0.005(4) -0.004(3) -0.010(4)
C1A 0.023(4) 0.039(6) 0.022(4) 0.007(4) 0.005(3) 0.000(4)
N1' 0.038(4) 0.026(5) 0.019(4) 0.004(3) -0.002(3) -0.001(3)
N2' 0.028(3) 0.022(4) 0.026(4) 0.004(3) 0.000(3) 0.002(3)
N3' 0.034(3) 0.029(5) 0.012(3) -0.001(4) 0.002(2) -0.003(3)
C4' 0.033(4) 0.028(6) 0.016(4) 0.001(4) 0.002(3) 0.000(4)
C5' 0.035(4) 0.031(6) 0.024(4) 0.002(5) 0.008(3) -0.002(4)
C6 0.022(4) 0.045(6) 0.015(4) 0.008(5) -0.003(3) -0.006(5)
C7 0.033(4) 0.054(7) 0.021(5) -0.007(5) -0.009(4) 0.008(4)
C8 0.025(4) 0.130(11) 0.016(5) 0.000(7) -0.004(3) -0.004(6)
C9 0.039(5) 0.112(11) 0.029(6) 0.013(7) -0.010(4) -0.035(6)
C10 0.064(6) 0.059(8) 0.044(6) 0.022(6) -0.020(5) -0.038(5)
C11 0.046(5) 0.041(7) 0.021(5) 0.000(5) -0.010(4) -0.009(5)
C12 0.059(6) 0.088(9) 0.036(5) -0.021(6) -0.005(4) 0.032(6)
C13 0.076(6) 0.190(13) 0.025(5) 0.035(6) -0.015(4) -0.084(7)
C14 0.092(7) 0.043(7) 0.046(6) 0.003(5) -0.005(5) -0.010(5)
C6' 0.048(5) 0.038(6) 0.027(5) -0.008(5) 0.001(4) 0.010(4)
C7' 0.061(6) 0.027(6) 0.024(5) -0.004(4) -0.002(4) 0.009(4)
C8' 0.064(5) 0.054(7) 0.030(5) 0.007(6) 0.001(4) 0.000(6)
C9' 0.106(8) 0.039(7) 0.035(5) 0.010(5) -0.003(5) -0.006(5)
C10' 0.104(8) 0.057(9) 0.025(5) 0.005(5) -0.023(5) 0.000(6)
C11' 0.085(7) 0.048(7) 0.033(5) -0.003(5) -0.018(5) 0.001(5)
C12' 0.072(6) 0.039(6) 0.024(4) 0.002(5) 0.000(4) 0.004(5)
C1B 0.029(4) 0.047(6) 0.025(4) 0.001(5) -0.004(3) -0.009(4)
O1B 0.032(3) 0.074(5) 0.025(3) 0.012(3) 0.002(2) 0.000(3)
C2B 0.029(4) 0.046(6) 0.029(4) -0.008(4) 0.005(3) -0.001(3)
O2B 0.035(3) 0.092(6) 0.051(4) -0.013(3) -0.005(2) -0.031(3)
B1D 0.028(5) 0.047(8) 0.029(5) 0.013(6) 0.004(4) 0.002(5)
C11D 0.027(4) 0.029(6) 0.032(4) 0.004(4) 0.007(3) -0.003(3)
C12D 0.040(4) 0.034(6) 0.025(4) 0.005(4) 0.008(3) 0.004(4)
C13D 0.030(4) 0.025(5) 0.041(5) -0.003(5) -0.004(3) 0.009(4)
C14D 0.039(5) 0.057(7) 0.022(4) 0.010(4) -0.010(3) 0.004(4)
C15D 0.043(5) 0.053(7) 0.028(4) 0.002(4) 0.001(4) -0.003(4)
C16D 0.036(4) 0.045(7) 0.035(4) 0.008(5) 0.000(4) -0.008(4)
C21D 0.030(5) 0.052(7) 0.038(5) 0.015(5) 0.010(4) -0.001(4)
C22D 0.025(5) 0.111(10) 0.043(5) -0.010(6) 0.006(4) 0.006(5)
C23D 0.039(6) 0.144(14) 0.050(6) -0.016(7) 0.004(5) 0.007(6)
C24D 0.027(6) 0.164(15) 0.037(6) 0.040(8) -0.005(4) 0.005(7)
C25D 0.039(6) 0.114(13) 0.086(8) 0.078(8) -0.021(5) -0.012(6)
C26D 0.031(5) 0.077(10) 0.085(7) 0.039(7) -0.003(4) 0.007(5)
C31D 0.028(4) 0.038(6) 0.033(4) 0.007(5) 0.003(3) -0.009(4)
C32D 0.042(5) 0.042(7) 0.043(5) 0.002(5) -0.009(4) 0.001(4)
C33D 0.051(5) 0.038(7) 0.049(6) 0.002(5) -0.017(4) -0.003(4)
C34D 0.061(5) 0.033(6) 0.040(5) -0.002(5) 0.007(5) -0.004(4)
C35D 0.042(5) 0.031(6) 0.049(5) 0.006(5) 0.006(4) -0.006(4)
C36D 0.043(5) 0.027(6) 0.028(5) 0.009(4) -0.001(4) -0.014(4)
C41D 0.026(4) 0.037(6) 0.030(5) -0.001(5) 0.012(3) 0.004(4)
C42D 0.037(4) 0.043(6) 0.030(5) 0.008(6) 0.003(3) -0.001(5)
C43D 0.052(5) 0.046(7) 0.060(6) 0.033(6) 0.005(4) -0.002(5)
C44D 0.048(5) 0.030(7) 0.065(7) -0.011(6) 0.002(5) 0.004(4)
C45D 0.046(5) 0.045(7) 0.037(5) -0.011(6) 0.015(4) 0.007(5)
C46D 0.035(4) 0.044(7) 0.039(5) 0.008(6) 0.019(3) 0.012(5)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 C1B 1.840(6) . ?
Rh1 C2B 1.888(7) . ?
Rh1 C2 2.053(6) . ?
Rh1 N3' 2.060(5) . ?
N1 C2 1.366(7) . ?
N1 C5 1.379(7) . ?
N1 C6 1.456(8) . ?
C2 N3 1.348(7) . ?
N3 C4 1.384(7) . ?
N3 C1A 1.472(7) . ?
C4 C5 1.344(8) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C1A C4' 1.482(9) . ?
C1A H1A1 0.9900 . ?
C1A H1A2 0.9900 . ?
N1' N2' 1.330(6) . ?
N1' C5' 1.346(8) . ?
N1' C6' 1.474(8) . ?
N2' N3' 1.328(6) . ?
N3' C4' 1.359(7) . ?
C4' C5' 1.352(8) . ?
C5' H5' 0.9500 . ?
C6 C7 1.385(10) . ?
C6 C11 1.390(10) . ?
C7 C8 1.409(10) . ?
C7 C12 1.485(11) . ?
C8 C9 1.381(13) . ?
C8 H8 0.9500 . ?
C9 C10 1.379(12) . ?
C9 C13 1.500(10) . ?
C10 C11 1.399(10) . ?
C10 H10 0.9500 . ?
C11 C14 1.485(10) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C6' C7' 1.524(9) . ?
C6' H6'1 0.9900 . ?
C6' H6'2 0.9900 . ?
C7' C8' 1.378(10) . ?
C7' C12' 1.378(9) . ?
C8' C9' 1.405(10) . ?
C8' H8' 0.9500 . ?
C9' C10' 1.371(9) . ?
C9' H9' 0.9500 . ?
C10' C11' 1.373(11) . ?
C10' H10' 0.9500 . ?
C11' C12' 1.391(9) . ?
C11' H11' 0.9500 . ?
C12' H12' 0.9500 . ?
C1B O1B 1.154(6) . ?
C2B O2B 1.136(6) . ?
B1D C41D 1.619(12) . ?
B1D C31D 1.641(11) . ?
B1D C21D 1.655(9) . ?
B1D C11D 1.662(10) . ?
C11D C16D 1.388(8) . ?
C11D C12D 1.407(7) . ?
C12D C13D 1.389(8) . ?
C12D H12D 0.9500 . ?
C13D C14D 1.370(8) . ?
C13D H13D 0.9500 . ?
C14D C15D 1.387(8) . ?
C14D H14D 0.9500 . ?
C15D C16D 1.386(8) . ?
C15D H15D 0.9500 . ?
C16D H16D 0.9500 . ?
C21D C26D 1.387(11) . ?
C21D C22D 1.388(11) . ?
C22D C23D 1.397(9) . ?
C22D H22D 0.9500 . ?
C23D C24D 1.354(15) . ?
C23D H23D 0.9500 . ?
C24D C25D 1.374(14) . ?
C24D H24D 0.9500 . ?
C25D C26D 1.414(10) . ?
C25D H25D 0.9500 . ?
C26D H26D 0.9500 . ?
C31D C36D 1.404(9) . ?
C31D C32D 1.413(8) . ?
C32D C33D 1.367(9) . ?
C32D H32D 0.9500 . ?
C33D C34D 1.383(9) . ?
C33D H33D 0.9500 . ?
C34D C35D 1.387(9) . ?
C34D H34D 0.9500 . ?
C35D C36D 1.387(9) . ?
C35D H35D 0.9500 . ?
C36D H36D 0.9500 . ?
C41D C42D 1.388(9) . ?
C41D C46D 1.399(9) . ?
C42D C43D 1.407(11) . ?
C42D H42D 0.9500 . ?
C43D C44D 1.395(10) . ?
C43D H43D 0.9500 . ?
C44D C45D 1.377(9) . ?
C44D H44D 0.9500 . ?
C45D C46D 1.388(10) . ?
C45D H45D 0.9500 . ?
C46D H46D 0.9500 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1B Rh1 C2B 88.4(3) . . ?
C1B Rh1 C2 94.9(3) . . ?
C2B Rh1 C2 174.3(3) . . ?
C1B Rh1 N3' 178.2(3) . . ?
C2B Rh1 N3' 90.2(2) . . ?
C2 Rh1 N3' 86.4(2) . . ?
C2 N1 C5 111.7(5) . . ?
C2 N1 C6 125.5(5) . . ?
C5 N1 C6 122.6(5) . . ?
N3 C2 N1 102.5(5) . . ?
N3 C2 Rh1 126.6(4) . . ?
N1 C2 Rh1 130.8(5) . . ?
C2 N3 C4 113.2(5) . . ?
C2 N3 C1A 125.5(5) . . ?
C4 N3 C1A 121.2(5) . . ?
C5 C4 N3 105.3(6) . . ?
C5 C4 H4 127.3 . . ?
N3 C4 H4 127.3 . . ?
C4 C5 N1 107.2(6) . . ?
C4 C5 H5 126.4 . . ?
N1 C5 H5 126.4 . . ?
N3 C1A C4' 112.9(6) . . ?
N3 C1A H1A1 109.0 . . ?
C4' C1A H1A1 109.0 . . ?
N3 C1A H1A2 109.0 . . ?
C4' C1A H1A2 109.0 . . ?
H1A1 C1A H1A2 107.8 . . ?
N2' N1' C5' 112.4(6) . . ?
N2' N1' C6' 120.4(6) . . ?
C5' N1' C6' 127.2(6) . . ?
N3' N2' N1' 105.0(5) . . ?
N2' N3' C4' 110.2(5) . . ?
N2' N3' Rh1 121.5(4) . . ?
C4' N3' Rh1 127.6(4) . . ?
C5' C4' N3' 107.5(6) . . ?
C5' C4' C1A 129.6(6) . . ?
N3' C4' C1A 122.9(6) . . ?
N1' C5' C4' 105.0(6) . . ?
N1' C5' H5' 127.5 . . ?
C4' C5' H5' 127.5 . . ?
C7 C6 C11 123.8(7) . . ?
C7 C6 N1 118.4(8) . . ?
C11 C6 N1 117.8(7) . . ?
C6 C7 C8 116.1(9) . . ?
C6 C7 C12 121.8(8) . . ?
C8 C7 C12 122.1(8) . . ?
C9 C8 C7 123.1(9) . . ?
C9 C8 H8 118.4 . . ?
C7 C8 H8 118.4 . . ?
C10 C9 C8 117.4(9) . . ?
C10 C9 C13 121.7(11) . . ?
C8 C9 C13 120.9(10) . . ?
C9 C10 C11 123.2(10) . . ?
C9 C10 H10 118.4 . . ?
C11 C10 H10 118.4 . . ?
C6 C11 C10 116.4(8) . . ?
C6 C11 C14 122.5(7) . . ?
C10 C11 C14 121.1(9) . . ?
C7 C12 H12A 109.5 . . ?
C7 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C7 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C9 C13 H13A 109.5 . . ?
C9 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C9 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N1' C6' C7' 113.6(6) . . ?
N1' C6' H6'1 108.8 . . ?
C7' C6' H6'1 108.8 . . ?
N1' C6' H6'2 108.8 . . ?
C7' C6' H6'2 108.8 . . ?
H6'1 C6' H6'2 107.7 . . ?
C8' C7' C12' 119.9(7) . . ?
C8' C7' C6' 119.9(7) . . ?
C12' C7' C6' 120.2(8) . . ?
C7' C8' C9' 119.5(7) . . ?
C7' C8' H8' 120.2 . . ?
C9' C8' H8' 120.2 . . ?
C10' C9' C8' 120.3(8) . . ?
C10' C9' H9' 119.9 . . ?
C8' C9' H9' 119.9 . . ?
C9' C10' C11' 119.8(8) . . ?
C9' C10' H10' 120.1 . . ?
C11' C10' H10' 120.1 . . ?
C10' C11' C12' 120.4(8) . . ?
C10' C11' H11' 119.8 . . ?
C12' C11' H11' 119.8 . . ?
C7' C12' C11' 120.0(8) . . ?
C7' C12' H12' 120.0 . . ?
C11' C12' H12' 120.0 . . ?
O1B C1B Rh1 172.4(5) . . ?
O2B C2B Rh1 177.6(6) . . ?
C41D B1D C31D 112.2(6) . . ?
C41D B1D C21D 108.6(7) . . ?
C31D B1D C21D 108.0(6) . . ?
C41D B1D C11D 108.1(6) . . ?
C31D B1D C11D 110.1(6) . . ?
C21D B1D C11D 109.9(6) . . ?
C16D C11D C12D 114.9(6) . . ?
C16D C11D B1D 125.7(6) . . ?
C12D C11D B1D 119.2(6) . . ?
C13D C12D C11D 122.8(6) . . ?
C13D C12D H12D 118.6 . . ?
C11D C12D H12D 118.6 . . ?
C14D C13D C12D 119.9(6) . . ?
C14D C13D H13D 120.0 . . ?
C12D C13D H13D 120.0 . . ?
C13D C14D C15D 119.5(6) . . ?
C13D C14D H14D 120.2 . . ?
C15D C14D H14D 120.2 . . ?
C16D C15D C14D 119.4(6) . . ?
C16D C15D H15D 120.3 . . ?
C14D C15D H15D 120.3 . . ?
C15D C16D C11D 123.5(6) . . ?
C15D C16D H16D 118.3 . . ?
C11D C16D H16D 118.3 . . ?
C26D C21D C22D 115.7(7) . . ?
C26D C21D B1D 121.8(8) . . ?
C22D C21D B1D 122.5(8) . . ?
C21D C22D C23D 122.4(9) . . ?
C21D C22D H22D 118.8 . . ?
C23D C22D H22D 118.8 . . ?
C24D C23D C22D 119.7(11) . . ?
C24D C23D H23D 120.2 . . ?
C22D C23D H23D 120.2 . . ?
C23D C24D C25D 121.4(10) . . ?
C23D C24D H24D 119.3 . . ?
C25D C24D H24D 119.3 . . ?
C24D C25D C26D 117.6(11) . . ?
C24D C25D H25D 121.2 . . ?
C26D C25D H25D 121.2 . . ?
C21D C26D C25D 123.1(9) . . ?
C21D C26D H26D 118.5 . . ?
C25D C26D H26D 118.5 . . ?
C36D C31D C32D 114.0(6) . . ?
C36D C31D B1D 126.7(6) . . ?
C32D C31D B1D 119.3(7) . . ?
C33D C32D C31D 122.7(7) . . ?
C33D C32D H32D 118.7 . . ?
C31D C32D H32D 118.7 . . ?
C32D C33D C34D 122.3(7) . . ?
C32D C33D H33D 118.8 . . ?
C34D C33D H33D 118.8 . . ?
C33D C34D C35D 116.9(7) . . ?
C33D C34D H34D 121.6 . . ?
C35D C34D H34D 121.6 . . ?
C36D C35D C34D 120.9(7) . . ?
C36D C35D H35D 119.6 . . ?
C34D C35D H35D 119.6 . . ?
C35D C36D C31D 123.3(7) . . ?
C35D C36D H36D 118.4 . . ?
C31D C36D H36D 118.4 . . ?
C42D C41D C46D 115.2(8) . . ?
C42D C41D B1D 124.5(7) . . ?
C46D C41D B1D 120.2(7) . . ?
C41D C42D C43D 123.4(8) . . ?
C41D C42D H42D 118.3 . . ?
C43D C42D H42D 118.3 . . ?
C44D C43D C42D 119.0(8) . . ?
C44D C43D H43D 120.5 . . ?
C42D C43D H43D 120.5 . . ?
C45D C44D C43D 118.9(8) . . ?
C45D C44D H44D 120.6 . . ?
C43D C44D H44D 120.6 . . ?
C44D C45D C46D 120.8(8) . . ?
C44D C45D H45D 119.6 . . ?
C46D C45D H45D 119.6 . . ?
C45D C46D C41D 122.7(8) . . ?
C45D C46D H46D 118.7 . . ?
C41D C46D H46D 118.7 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 C2 N3 0.5(7) . . . . ?
C6 N1 C2 N3 -174.9(7) . . . . ?
C5 N1 C2 Rh1 -179.5(5) . . . . ?
C6 N1 C2 Rh1 5.1(10) . . . . ?
C1B Rh1 C2 N3 -158.3(6) . . . . ?
C2B Rh1 C2 N3 77(3) . . . . ?
N3' Rh1 C2 N3 23.0(6) . . . . ?
C1B Rh1 C2 N1 21.7(7) . . . . ?
C2B Rh1 C2 N1 -103(3) . . . . ?
N3' Rh1 C2 N1 -157.0(7) . . . . ?
N1 C2 N3 C4 -1.0(7) . . . . ?
Rh1 C2 N3 C4 179.0(5) . . . . ?
N1 C2 N3 C1A -178.6(6) . . . . ?
Rh1 C2 N3 C1A 1.4(10) . . . . ?
C2 N3 C4 C5 1.2(8) . . . . ?
C1A N3 C4 C5 178.8(6) . . . . ?
N3 C4 C5 N1 -0.8(8) . . . . ?
C2 N1 C5 C4 0.2(9) . . . . ?
C6 N1 C5 C4 175.8(7) . . . . ?
C2 N3 C1A C4' -39.3(9) . . . . ?
C4 N3 C1A C4' 143.3(6) . . . . ?
C5' N1' N2' N3' -0.3(7) . . . . ?
C6' N1' N2' N3' 179.4(5) . . . . ?
N1' N2' N3' C4' 0.9(7) . . . . ?
N1' N2' N3' Rh1 -170.4(4) . . . . ?
C1B Rh1 N3' N2' 19(8) . . . . ?
C2B Rh1 N3' N2' -23.2(5) . . . . ?
C2 Rh1 N3' N2' 152.2(5) . . . . ?
C1B Rh1 N3' C4' -151(8) . . . . ?
C2B Rh1 N3' C4' 167.2(6) . . . . ?
C2 Rh1 N3' C4' -17.3(6) . . . . ?
N2' N3' C4' C5' -1.1(8) . . . . ?
Rh1 N3' C4' C5' 169.5(5) . . . . ?
N2' N3' C4' C1A 176.4(6) . . . . ?
Rh1 N3' C4' C1A -13.0(10) . . . . ?
N3 C1A C4' C5' -138.1(7) . . . . ?
N3 C1A C4' N3' 44.9(9) . . . . ?
N2' N1' C5' C4' -0.3(8) . . . . ?
C6' N1' C5' C4' 180.0(6) . . . . ?
N3' C4' C5' N1' 0.8(8) . . . . ?
C1A C4' C5' N1' -176.4(7) . . . . ?
C2 N1 C6 C7 -100.7(8) . . . . ?
C5 N1 C6 C7 84.4(8) . . . . ?
C2 N1 C6 C11 81.3(8) . . . . ?
C5 N1 C6 C11 -93.6(8) . . . . ?
C11 C6 C7 C8 -3.4(9) . . . . ?
N1 C6 C7 C8 178.7(5) . . . . ?
C11 C6 C7 C12 178.1(6) . . . . ?
N1 C6 C7 C12 0.2(9) . . . . ?
C6 C7 C8 C9 0.6(10) . . . . ?
C12 C7 C8 C9 179.1(7) . . . . ?
C7 C8 C9 C10 1.7(12) . . . . ?
C7 C8 C9 C13 -177.6(6) . . . . ?
C8 C9 C10 C11 -1.5(12) . . . . ?
C13 C9 C10 C11 177.9(6) . . . . ?
C7 C6 C11 C10 3.6(10) . . . . ?
N1 C6 C11 C10 -178.5(5) . . . . ?
C7 C6 C11 C14 -173.8(6) . . . . ?
N1 C6 C11 C14 4.1(10) . . . . ?
C9 C10 C11 C6 -1.1(11) . . . . ?
C9 C10 C11 C14 176.4(7) . . . . ?
N2' N1' C6' C7' 95.5(7) . . . . ?
C5' N1' C6' C7' -84.8(8) . . . . ?
N1' C6' C7' C8' 63.5(9) . . . . ?
N1' C6' C7' C12' -116.6(8) . . . . ?
C12' C7' C8' C9' 0.5(12) . . . . ?
C6' C7' C8' C9' -179.5(7) . . . . ?
C7' C8' C9' C10' -0.7(12) . . . . ?
C8' C9' C10' C11' 1.0(13) . . . . ?
C9' C10' C11' C12' -1.0(13) . . . . ?
C8' C7' C12' C11' -0.6(11) . . . . ?
C6' C7' C12' C11' 179.5(7) . . . . ?
C10' C11' C12' C7' 0.8(12) . . . . ?
C2B Rh1 C1B O1B -27(6) . . . . ?
C2 Rh1 C1B O1B 157(6) . . . . ?
N3' Rh1 C1B O1B -69(12) . . . . ?
C1B Rh1 C2B O2B -30(17) . . . . ?
C2 Rh1 C2B O2B 96(17) . . . . ?
N3' Rh1 C2B O2B 149(17) . . . . ?
C41D B1D C11D C16D -117.8(8) . . . . ?
C31D B1D C11D C16D 119.4(8) . . . . ?
C21D B1D C11D C16D 0.6(11) . . . . ?
C41D B1D C11D C12D 56.4(8) . . . . ?
C31D B1D C11D C12D -66.4(9) . . . . ?
C21D B1D C11D C12D 174.8(6) . . . . ?
C16D C11D C12D C13D -1.1(10) . . . . ?
B1D C11D C12D C13D -175.9(7) . . . . ?
C11D C12D C13D C14D 0.7(11) . . . . ?
C12D C13D C14D C15D -0.1(11) . . . . ?
C13D C14D C15D C16D -0.1(11) . . . . ?
C14D C15D C16D C11D -0.3(12) . . . . ?
C12D C11D C16D C15D 0.9(11) . . . . ?
B1D C11D C16D C15D 175.3(8) . . . . ?
C41D B1D C21D C26D -167.2(7) . . . . ?
C31D B1D C21D C26D -45.3(9) . . . . ?
C11D B1D C21D C26D 74.8(9) . . . . ?
C41D B1D C21D C22D 11.0(9) . . . . ?
C31D B1D C21D C22D 133.0(8) . . . . ?
C11D B1D C21D C22D -107.0(8) . . . . ?
C26D C21D C22D C23D -3.7(11) . . . . ?
B1D C21D C22D C23D 177.9(7) . . . . ?
C21D C22D C23D C24D 0.4(13) . . . . ?
C22D C23D C24D C25D 2.1(14) . . . . ?
C23D C24D C25D C26D -1.1(14) . . . . ?
C22D C21D C26D C25D 4.9(11) . . . . ?
B1D C21D C26D C25D -176.7(6) . . . . ?
C24D C25D C26D C21D -2.6(12) . . . . ?
C41D B1D C31D C36D -104.7(8) . . . . ?
C21D B1D C31D C36D 135.6(7) . . . . ?
C11D B1D C31D C36D 15.6(10) . . . . ?
C41D B1D C31D C32D 74.8(8) . . . . ?
C21D B1D C31D C32D -44.9(9) . . . . ?
C11D B1D C31D C32D -164.9(6) . . . . ?
C36D C31D C32D C33D -0.7(10) . . . . ?
B1D C31D C32D C33D 179.8(7) . . . . ?
C31D C32D C33D C34D 0.5(12) . . . . ?
C32D C33D C34D C35D 0.8(11) . . . . ?
C33D C34D C35D C36D -1.8(11) . . . . ?
C34D C35D C36D C31D 1.7(11) . . . . ?
C32D C31D C36D C35D -0.4(10) . . . . ?
B1D C31D C36D C35D 179.1(7) . . . . ?
C31D B1D C41D C42D -25.4(9) . . . . ?
C21D B1D C41D C42D 93.9(7) . . . . ?
C11D B1D C41D C42D -146.9(6) . . . . ?
C31D B1D C41D C46D 158.0(6) . . . . ?
C21D B1D C41D C46D -82.7(7) . . . . ?
C11D B1D C41D C46D 36.4(8) . . . . ?
C46D C41D C42D C43D -0.7(9) . . . . ?
B1D C41D C42D C43D -177.5(6) . . . . ?
C41D C42D C43D C44D 1.2(11) . . . . ?
C42D C43D C44D C45D -0.2(10) . . . . ?
C43D C44D C45D C46D -1.1(10) . . . . ?
C44D C45D C46D C41D 1.7(10) . . . . ?
C42D C41D C46D C45D -0.8(9) . . . . ?
B1D C41D C46D C45D 176.2(6) . . . . ?
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max 0.458
_refine_diff_density_min -0.675
_refine_diff_density_rms 0.108
_database_code_depnum_ccdc_archive 'CCDC 934036'
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_inp1bar2
#TrackingRef 'Khuong4_Deposition_15May12.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C30 H34 N6 O2 Rh, C24 H20 B'
_chemical_formula_sum 'C54 H54 B N6 O2 Rh'
_chemical_formula_weight 932.75
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Triclinic
_symmetry_space_group_name_H-M P-1
_symmetry_space_group_name_Hall '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 11.0520(5)
_cell_length_b 15.3218(6)
_cell_length_c 15.4565(7)
_cell_angle_alpha 113.899(2)
_cell_angle_beta 90.403(2)
_cell_angle_gamma 101.927(2)
_cell_volume 2329.20(17)
_cell_formula_units_Z 2
_cell_measurement_temperature 150(2)
_cell_measurement_reflns_used 5649
_cell_measurement_theta_min 2.126
_cell_measurement_theta_max 23.142
_exptl_crystal_description Plates
_exptl_crystal_colour Yellow
_exptl_crystal_size_max 0.21
_exptl_crystal_size_mid 0.19
_exptl_crystal_size_min 0.04
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.330
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 972
_exptl_absorpt_coefficient_mu 0.415
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.9172
_exptl_absorpt_correction_T_max 0.9828
_exptl_absorpt_process_details 'SADABS (Bruker, 2001)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 150(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker kappa APEXII CCD Diffractometer'
_diffrn_measurement_method '\f scans, and \w scans with \k offsets'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 31253
_diffrn_reflns_av_R_equivalents 0.0584
_diffrn_reflns_av_sigmaI/netI 0.0597
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_theta_min 2.26
_diffrn_reflns_theta_max 25.00
_reflns_number_total 8091
_reflns_number_gt 6144
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2007)'
_computing_cell_refinement 'APEX2 (Bruker, 2007)'
_computing_data_reduction 'APEX2 (Bruker, 2007)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
Two of the phenyl rings (C31D-C36D and C41D-C46D) of the anion (BPh4)
exhibited large thermal anisotropies, reaching the maximum values for
the tip atoms of the rings. These rings were constrained to regular
six membered rings using command AFIX 66 in SHELXL.The nitro group
(N4'/O1'/O2') also showed slightly higher atomic displacement parameters
than the bonded neighbouring carbon C10'. The final difference electron
density contained a peak of ~ 1.4 eA-3, which is a ripple around the heavy
metal ion Rh1. The alerts at level B and some at level C are because of
the above features in the refinement.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0519P)^2^+4.0793P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 8091
_refine_ls_number_parameters 556
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0766
_refine_ls_R_factor_gt 0.0512
_refine_ls_wR_factor_ref 0.1299
_refine_ls_wR_factor_gt 0.1163
_refine_ls_goodness_of_fit_ref 1.030
_refine_ls_restrained_S_all 1.030
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.78060(3) 0.69317(2) 0.64695(3) 0.03363(12) Uani 1 1 d . . .
N1 N 0.8277(3) 0.9163(2) 0.7910(2) 0.0312(8) Uani 1 1 d . . .
C2 C 0.7725(4) 0.8194(3) 0.7625(3) 0.0334(10) Uani 1 1 d . . .
N3 N 0.7096(3) 0.8179(2) 0.8367(3) 0.0353(8) Uani 1 1 d . . .
C4 C 0.7243(4) 0.9099(3) 0.9094(3) 0.0385(10) Uani 1 1 d . . .
H4 H 0.6883 0.9261 0.9680 0.046 Uiso 1 1 calc R . .
C5 C 0.7993(4) 0.9722(3) 0.8813(3) 0.0368(10) Uani 1 1 d . . .
H5 H 0.8275 1.0410 0.9164 0.044 Uiso 1 1 calc R . .
C1A C 0.6340(4) 0.7279(3) 0.8390(4) 0.0440(11) Uani 1 1 d . . .
H1A1 H 0.5613 0.7017 0.7906 0.053 Uiso 1 1 calc R . .
H1A2 H 0.6029 0.7435 0.9022 0.053 Uiso 1 1 calc R . .
N1' N 0.7956(4) 0.5376(3) 0.8133(3) 0.0421(9) Uani 1 1 d . . .
N2' N 0.8323(3) 0.5600(2) 0.7410(3) 0.0408(9) Uani 1 1 d . . .
N3' N 0.7780(3) 0.6310(2) 0.7449(3) 0.0370(8) Uani 1 1 d . . .
C4' C 0.7079(4) 0.6520(3) 0.8197(3) 0.0394(11) Uani 1 1 d . . .
C5' C 0.7192(4) 0.5926(3) 0.8634(3) 0.0446(11) Uani 1 1 d . . .
H5' H 0.6812 0.5905 0.9177 0.054 Uiso 1 1 calc R . .
C6 C 0.9108(4) 0.9585(3) 0.7385(3) 0.0332(9) Uani 1 1 d . . .
C7 C 0.8665(4) 1.0104(3) 0.6948(3) 0.0422(11) Uani 1 1 d . . .
C8 C 0.9539(6) 1.0528(3) 0.6481(3) 0.0548(15) Uani 1 1 d . . .
H8 H 0.9272 1.0892 0.6174 0.066 Uiso 1 1 calc R . .
C9 C 1.0742(5) 1.0441(3) 0.6449(3) 0.0515(13) Uani 1 1 d . . .
C10 C 1.1122(5) 0.9901(3) 0.6882(3) 0.0474(12) Uani 1 1 d . . .
H6B H 1.1950 0.9817 0.6845 0.057 Uiso 1 1 calc R . .
C11 C 1.0329(4) 0.9473(3) 0.7374(3) 0.0366(10) Uani 1 1 d . . .
C12 C 0.7357(5) 1.0230(4) 0.6983(4) 0.0587(14) Uani 1 1 d . . .
H12A H 0.6785 0.9600 0.6852 0.088 Uiso 1 1 calc R . .
H12B H 0.7168 1.0463 0.6504 0.088 Uiso 1 1 calc R . .
H12C H 0.7262 1.0711 0.7616 0.088 Uiso 1 1 calc R . .
C13 C 1.1643(7) 1.0938(4) 0.5963(4) 0.078(2) Uani 1 1 d . . .
H13A H 1.2058 1.1597 0.6425 0.117 Uiso 1 1 calc R . .
H13B H 1.1187 1.0986 0.5444 0.117 Uiso 1 1 calc R . .
H13C H 1.2265 1.0553 0.5706 0.117 Uiso 1 1 calc R . .
C14 C 1.0778(4) 0.8910(4) 0.7849(4) 0.0493(12) Uani 1 1 d . . .
H14A H 1.0572 0.9149 0.8509 0.074 Uiso 1 1 calc R . .
H14B H 1.1681 0.8996 0.7841 0.074 Uiso 1 1 calc R . .
H14C H 1.0375 0.8212 0.7510 0.074 Uiso 1 1 calc R . .
C6' C 0.8328(5) 0.4540(3) 0.8225(4) 0.0518(13) Uani 1 1 d . . .
H6'1 H 0.8127 0.4532 0.8845 0.062 Uiso 1 1 calc R . .
H6'2 H 0.9235 0.4609 0.8195 0.062 Uiso 1 1 calc R . .
C7' C 0.7648(4) 0.3605(3) 0.7434(3) 0.0396(10) Uani 1 1 d . . .
C8' C 0.6483(5) 0.3133(4) 0.7489(4) 0.0587(14) Uani 1 1 d . . .
H8' H 0.6114 0.3363 0.8069 0.070 Uiso 1 1 calc R . .
C9' C 0.5814(5) 0.2305(4) 0.6693(4) 0.0610(14) Uani 1 1 d . . .
H9' H 0.4991 0.1982 0.6718 0.073 Uiso 1 1 calc R . .
C10' C 0.6404(5) 0.1995(4) 0.5894(4) 0.0504(12) Uani 1 1 d . . .
C11' C 0.7606(6) 0.2399(4) 0.5838(4) 0.0728(17) Uani 1 1 d . . .
H11' H 0.8007 0.2123 0.5282 0.087 Uiso 1 1 calc R . .
C12' C 0.8214(6) 0.3214(4) 0.6608(4) 0.0683(16) Uani 1 1 d . . .
H12' H 0.9043 0.3520 0.6579 0.082 Uiso 1 1 calc R . .
N4' N 0.5685(7) 0.1151(4) 0.5051(4) 0.0788(16) Uani 1 1 d . . .
O1' O 0.4556(5) 0.0909(4) 0.5050(4) 0.0973(16) Uani 1 1 d . . .
O2' O 0.6286(6) 0.0737(3) 0.4384(3) 0.1063(18) Uani 1 1 d . . .
C1B C 0.6916(4) 0.7341(3) 0.5502(3) 0.0408(11) Uani 1 1 d . . .
H1B H 0.6620 0.7807 0.6024 0.049 Uiso 1 1 calc R . .
C2B C 0.8169(4) 0.7534(3) 0.5433(3) 0.0392(10) Uani 1 1 d . . .
H2B H 0.8673 0.8094 0.5933 0.047 Uiso 1 1 calc R . .
C3B C 0.8818(4) 0.6921(3) 0.4615(3) 0.0474(12) Uani 1 1 d . . .
H3B1 H 0.9527 0.7359 0.4499 0.057 Uiso 1 1 calc R . .
H3B2 H 0.8229 0.6594 0.4030 0.057 Uiso 1 1 calc R . .
C4B C 0.9293(5) 0.6140(4) 0.4813(4) 0.0521(13) Uani 1 1 d . . .
H4B1 H 0.9346 0.5595 0.4199 0.062 Uiso 1 1 calc R . .
H4B2 H 1.0144 0.6431 0.5146 0.062 Uiso 1 1 calc R . .
C5B C 0.8490(4) 0.5732(3) 0.5404(3) 0.0429(11) Uani 1 1 d . . .
H5B H 0.8896 0.5645 0.5897 0.051 Uiso 1 1 calc R . .
C6B C 0.7200(4) 0.5471(3) 0.5283(3) 0.0434(11) Uani 1 1 d . . .
H6B1 H 0.6786 0.5256 0.5723 0.052 Uiso 1 1 calc R . .
C7B C 0.6413(4) 0.5505(3) 0.4507(3) 0.0478(12) Uani 1 1 d . . .
H7B1 H 0.5683 0.4943 0.4294 0.057 Uiso 1 1 calc R . .
H7B2 H 0.6900 0.5438 0.3958 0.057 Uiso 1 1 calc R . .
C8B C 0.5963(4) 0.6461(3) 0.4831(3) 0.0477(12) Uani 1 1 d . . .
H8B1 H 0.5751 0.6570 0.4265 0.057 Uiso 1 1 calc R . .
H8B2 H 0.5197 0.6394 0.5149 0.057 Uiso 1 1 calc R . .
B1D B 0.7195(4) 0.3022(3) 0.0763(3) 0.0312(10) Uani 1 1 d . . .
C11D C 0.7528(4) 0.4228(3) 0.1145(3) 0.0287(9) Uani 1 1 d . . .
C12D C 0.6838(4) 0.4806(3) 0.1798(3) 0.0363(10) Uani 1 1 d . . .
H12D H 0.6189 0.4496 0.2048 0.044 Uiso 1 1 calc R . .
C13D C 0.7059(5) 0.5817(3) 0.2098(3) 0.0453(11) Uani 1 1 d . . .
H13D H 0.6565 0.6183 0.2541 0.054 Uiso 1 1 calc R . .
C14D C 0.8004(5) 0.6288(3) 0.1747(3) 0.0470(12) Uani 1 1 d . . .
H14D H 0.8178 0.6980 0.1962 0.056 Uiso 1 1 calc R . .
C15D C 0.8689(4) 0.5746(3) 0.1084(4) 0.0475(12) Uani 1 1 d . . .
H15D H 0.9321 0.6060 0.0825 0.057 Uiso 1 1 calc R . .
C16D C 0.8451(4) 0.4736(3) 0.0795(3) 0.0366(10) Uani 1 1 d . . .
H16D H 0.8937 0.4374 0.0340 0.044 Uiso 1 1 calc R . .
C21D C 0.8370(4) 0.2596(3) 0.0250(3) 0.0313(9) Uani 1 1 d . . .
C22D C 0.9267(4) 0.2384(3) 0.0715(3) 0.0408(11) Uani 1 1 d . . .
H22D H 0.9185 0.2477 0.1357 0.049 Uiso 1 1 calc R . .
C23D C 1.0274(4) 0.2043(3) 0.0295(4) 0.0530(13) Uani 1 1 d . . .
H23D H 1.0854 0.1895 0.0641 0.064 Uiso 1 1 calc R . .
C24D C 1.0434(4) 0.1920(3) -0.0623(4) 0.0546(15) Uani 1 1 d . . .
H24D H 1.1127 0.1691 -0.0916 0.065 Uiso 1 1 calc R . .
C25D C 0.9577(4) 0.2132(3) -0.1116(3) 0.0474(12) Uani 1 1 d . . .
H25D H 0.9687 0.2063 -0.1748 0.057 Uiso 1 1 calc R . .
C26D C 0.8558(4) 0.2446(3) -0.0690(3) 0.0361(10) Uani 1 1 d . . .
H26D H 0.7961 0.2564 -0.1050 0.043 Uiso 1 1 calc R . .
C41D C 0.6934(3) 0.2732(2) 0.1697(2) 0.0433(11) Uani 1 1 d G . .
C42D C 0.6081(3) 0.1884(2) 0.1601(3) 0.0686(18) Uani 1 1 d G . .
H42D H 0.5642 0.1452 0.0998 0.082 Uiso 1 1 calc R . .
C43D C 0.5870(4) 0.1669(3) 0.2386(4) 0.118(4) Uani 1 1 d G . .
H43D H 0.5287 0.1090 0.2320 0.141 Uiso 1 1 calc R . .
C44D C 0.6512(5) 0.2301(4) 0.3268(3) 0.141(5) Uani 1 1 d G . .
H44D H 0.6368 0.2154 0.3804 0.169 Uiso 1 1 calc R . .
C45D C 0.7365(5) 0.3149(3) 0.3364(2) 0.110(3) Uani 1 1 d G . .
H45D H 0.7803 0.3581 0.3967 0.132 Uiso 1 1 calc R . .
C46D C 0.7576(3) 0.3364(2) 0.2579(2) 0.0666(17) Uani 1 1 d G . .
H46D H 0.8159 0.3943 0.2645 0.080 Uiso 1 1 calc R . .
C31D C 0.5949(2) 0.2568(2) -0.0057(2) 0.0453(12) Uani 1 1 d G . .
C32D C 0.5594(3) 0.1561(2) -0.0599(3) 0.079(2) Uani 1 1 d G . .
H32D H 0.6062 0.1141 -0.0516 0.095 Uiso 1 1 calc R . .
C33D C 0.4552(3) 0.1170(2) -0.1261(3) 0.117(3) Uani 1 1 d G . .
H33D H 0.4309 0.0482 -0.1631 0.140 Uiso 1 1 calc R . .
C34D C 0.3867(3) 0.1785(3) -0.1381(2) 0.107(3) Uani 1 1 d G . .
H34D H 0.3155 0.1517 -0.1834 0.128 Uiso 1 1 calc R . .
C35D C 0.4222(3) 0.2791(3) -0.0840(3) 0.0752(19) Uani 1 1 d G . .
H35D H 0.3754 0.3212 -0.0922 0.090 Uiso 1 1 calc R . .
C36D C 0.5264(3) 0.3183(2) -0.0178(2) 0.0508(13) Uani 1 1 d G . .
H36D H 0.5507 0.3871 0.0192 0.061 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Rh1 0.02979(19) 0.02292(18) 0.0433(2) 0.00879(14) 0.00501(14) 0.00612(13)
N1 0.0265(17) 0.0232(17) 0.040(2) 0.0093(15) 0.0005(15) 0.0049(14)
C2 0.026(2) 0.028(2) 0.046(3) 0.015(2) 0.0037(19) 0.0063(17)
N3 0.0255(17) 0.0281(19) 0.053(2) 0.0162(17) 0.0104(17) 0.0079(15)
C4 0.034(2) 0.034(2) 0.046(3) 0.012(2) 0.014(2) 0.0136(19)
C5 0.032(2) 0.028(2) 0.045(3) 0.008(2) 0.006(2) 0.0095(19)
C1A 0.034(2) 0.032(2) 0.071(3) 0.025(2) 0.022(2) 0.009(2)
N1' 0.050(2) 0.036(2) 0.042(2) 0.0172(18) 0.0033(18) 0.0126(18)
N2' 0.039(2) 0.030(2) 0.050(2) 0.0113(18) 0.0003(18) 0.0121(16)
N3' 0.0330(19) 0.0273(19) 0.048(2) 0.0121(17) 0.0059(17) 0.0091(15)
C4' 0.031(2) 0.031(2) 0.060(3) 0.021(2) 0.015(2) 0.0073(19)
C5' 0.046(3) 0.036(3) 0.051(3) 0.017(2) 0.013(2) 0.011(2)
C6 0.035(2) 0.022(2) 0.033(2) 0.0068(18) -0.0006(19) -0.0037(17)
C7 0.058(3) 0.025(2) 0.030(2) 0.0026(19) -0.015(2) 0.001(2)
C8 0.102(5) 0.026(2) 0.027(2) 0.008(2) -0.012(3) 0.003(3)
C9 0.069(4) 0.037(3) 0.032(3) 0.008(2) 0.002(2) -0.007(3)
C10 0.047(3) 0.042(3) 0.036(3) 0.008(2) 0.003(2) -0.008(2)
C11 0.035(2) 0.033(2) 0.032(2) 0.0090(19) 0.0025(19) -0.0010(19)
C12 0.068(3) 0.039(3) 0.064(3) 0.015(3) -0.021(3) 0.016(3)
C13 0.116(5) 0.054(3) 0.046(3) 0.022(3) 0.013(3) -0.020(3)
C14 0.030(2) 0.062(3) 0.065(3) 0.036(3) 0.008(2) 0.011(2)
C6' 0.059(3) 0.046(3) 0.060(3) 0.027(3) 0.001(3) 0.023(2)
C7' 0.045(3) 0.037(2) 0.047(3) 0.024(2) 0.009(2) 0.016(2)
C8' 0.053(3) 0.068(4) 0.059(3) 0.026(3) 0.015(3) 0.021(3)
C9' 0.042(3) 0.077(4) 0.073(4) 0.041(3) 0.009(3) 0.010(3)
C10' 0.062(3) 0.045(3) 0.049(3) 0.025(2) 0.001(3) 0.011(3)
C11' 0.084(4) 0.053(3) 0.069(4) 0.016(3) 0.032(3) 0.008(3)
C12' 0.065(4) 0.049(3) 0.075(4) 0.014(3) 0.027(3) 0.003(3)
N4' 0.120(5) 0.055(3) 0.065(4) 0.033(3) -0.001(4) 0.011(3)
O1' 0.077(3) 0.085(3) 0.112(4) 0.032(3) -0.029(3) 0.001(3)
O2' 0.163(5) 0.065(3) 0.069(3) 0.018(2) 0.024(3) 0.002(3)
C1B 0.042(3) 0.036(2) 0.041(3) 0.012(2) 0.006(2) 0.012(2)
C2B 0.048(3) 0.030(2) 0.032(2) 0.0085(19) 0.000(2) 0.003(2)
C3B 0.045(3) 0.040(3) 0.045(3) 0.010(2) 0.012(2) 0.003(2)
C4B 0.045(3) 0.045(3) 0.056(3) 0.010(2) 0.018(2) 0.012(2)
C5B 0.047(3) 0.029(2) 0.046(3) 0.006(2) 0.012(2) 0.015(2)
C6B 0.047(3) 0.029(2) 0.044(3) 0.006(2) 0.009(2) 0.007(2)
C7B 0.047(3) 0.035(3) 0.045(3) 0.005(2) 0.003(2) -0.002(2)
C8B 0.038(3) 0.051(3) 0.048(3) 0.016(2) 0.000(2) 0.010(2)
B1D 0.029(2) 0.028(2) 0.036(3) 0.012(2) 0.004(2) 0.007(2)
C11D 0.030(2) 0.031(2) 0.029(2) 0.0144(18) -0.0005(17) 0.0107(18)
C12D 0.043(2) 0.035(2) 0.037(2) 0.019(2) 0.008(2) 0.014(2)
C13D 0.057(3) 0.042(3) 0.043(3) 0.017(2) 0.011(2) 0.026(2)
C14D 0.058(3) 0.031(2) 0.054(3) 0.017(2) 0.007(2) 0.015(2)
C15D 0.047(3) 0.038(3) 0.063(3) 0.026(2) 0.015(2) 0.011(2)
C16D 0.037(2) 0.032(2) 0.040(2) 0.013(2) 0.009(2) 0.0103(19)
C21D 0.028(2) 0.0183(19) 0.041(2) 0.0080(18) 0.0012(18) 0.0008(16)
C22D 0.034(2) 0.034(2) 0.050(3) 0.014(2) -0.002(2) 0.0055(19)
C23D 0.024(2) 0.044(3) 0.085(4) 0.022(3) -0.003(2) 0.004(2)
C24D 0.027(2) 0.031(3) 0.088(4) 0.008(3) 0.022(3) 0.004(2)
C25D 0.045(3) 0.029(2) 0.048(3) 0.001(2) 0.018(2) -0.004(2)
C26D 0.036(2) 0.024(2) 0.039(2) 0.0065(18) 0.0020(19) -0.0013(18)
C41D 0.046(3) 0.037(3) 0.062(3) 0.027(2) 0.024(2) 0.029(2)
C42D 0.041(3) 0.070(4) 0.139(6) 0.079(4) 0.036(3) 0.029(3)
C43D 0.075(5) 0.137(7) 0.245(11) 0.158(9) 0.092(7) 0.074(5)
C44D 0.212(11) 0.182(10) 0.177(9) 0.161(9) 0.151(9) 0.172(9)
C45D 0.227(10) 0.105(6) 0.055(4) 0.046(4) 0.049(5) 0.128(7)
C46D 0.132(5) 0.050(3) 0.036(3) 0.020(3) 0.022(3) 0.054(3)
C31D 0.026(2) 0.048(3) 0.045(3) 0.004(2) 0.011(2) 0.005(2)
C32D 0.031(3) 0.060(4) 0.093(4) -0.017(3) 0.010(3) -0.001(3)
C33D 0.037(3) 0.104(6) 0.109(6) -0.047(5) 0.001(4) -0.002(4)
C34D 0.030(3) 0.163(8) 0.057(4) -0.014(4) -0.001(3) -0.001(4)
C35D 0.041(3) 0.127(6) 0.048(3) 0.024(4) 0.002(3) 0.027(3)
C36D 0.032(2) 0.082(4) 0.037(3) 0.019(3) 0.006(2) 0.020(2)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 C2 2.053(4) . ?
Rh1 N3' 2.088(4) . ?
Rh1 C1B 2.142(4) . ?
Rh1 C2B 2.153(4) . ?
Rh1 C5B 2.192(4) . ?
Rh1 C6B 2.204(4) . ?
N1 C2 1.365(5) . ?
N1 C5 1.389(5) . ?
N1 C6 1.453(5) . ?
C2 N3 1.350(5) . ?
N3 C4 1.376(5) . ?
N3 C1A 1.472(5) . ?
C4 C5 1.342(6) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C1A C4' 1.491(6) . ?
C1A H1A1 0.9900 . ?
C1A H1A2 0.9900 . ?
N1' N2' 1.339(5) . ?
N1' C5' 1.340(6) . ?
N1' C6' 1.481(6) . ?
N2' N3' 1.328(5) . ?
N3' C4' 1.361(5) . ?
C4' C5' 1.359(6) . ?
C5' H5' 0.9500 . ?
C6 C7 1.386(6) . ?
C6 C11 1.394(6) . ?
C7 C8 1.417(7) . ?
C7 C12 1.496(7) . ?
C8 C9 1.363(8) . ?
C8 H8 0.9500 . ?
C9 C10 1.377(7) . ?
C9 C13 1.515(7) . ?
C10 C11 1.397(6) . ?
C10 H6B 0.9500 . ?
C11 C14 1.488(6) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C6' C7' 1.494(7) . ?
C6' H6'1 0.9900 . ?
C6' H6'2 0.9900 . ?
C7' C8' 1.361(7) . ?
C7' C12' 1.388(7) . ?
C8' C9' 1.415(8) . ?
C8' H8' 0.9500 . ?
C9' C10' 1.357(7) . ?
C9' H9' 0.9500 . ?
C10' C11' 1.364(8) . ?
C10' N4' 1.482(7) . ?
C11' C12' 1.366(8) . ?
C11' H11' 0.9500 . ?
C12' H12' 0.9500 . ?
N4' O1' 1.227(7) . ?
N4' O2' 1.248(7) . ?
C1B C2B 1.369(6) . ?
C1B C8B 1.506(6) . ?
C1B H1B 0.9500 . ?
C2B C3B 1.525(6) . ?
C2B H2B 0.9500 . ?
C3B C4B 1.535(7) . ?
C3B H3B1 0.9900 . ?
C3B H3B2 0.9900 . ?
C4B C5B 1.502(7) . ?
C4B H4B1 0.9900 . ?
C4B H4B2 0.9900 . ?
C5B C6B 1.389(6) . ?
C5B H5B 0.9500 . ?
C6B C7B 1.501(7) . ?
C6B H6B1 0.9500 . ?
C7B C8B 1.534(6) . ?
C7B H7B1 0.9900 . ?
C7B H7B2 0.9900 . ?
C8B H8B1 0.9900 . ?
C8B H8B2 0.9900 . ?
B1D C21D 1.638(6) . ?
B1D C11D 1.652(6) . ?
B1D C41D 1.685(5) . ?
B1D C31D 1.689(5) . ?
C11D C12D 1.397(6) . ?
C11D C16D 1.400(6) . ?
C12D C13D 1.391(6) . ?
C12D H12D 0.9500 . ?
C13D C14D 1.385(7) . ?
C13D H13D 0.9500 . ?
C14D C15D 1.376(6) . ?
C14D H14D 0.9500 . ?
C15D C16D 1.390(6) . ?
C15D H15D 0.9500 . ?
C16D H16D 0.9500 . ?
C21D C22D 1.385(6) . ?
C21D C26D 1.401(6) . ?
C22D C23D 1.381(6) . ?
C22D H22D 0.9500 . ?
C23D C24D 1.372(7) . ?
C23D H23D 0.9500 . ?
C24D C25D 1.379(7) . ?
C24D H24D 0.9500 . ?
C25D C26D 1.382(6) . ?
C25D H25D 0.9500 . ?
C26D H26D 0.9500 . ?
C41D C42D 1.3900 . ?
C41D C46D 1.3900 . ?
C42D C43D 1.3900 . ?
C42D H42D 0.9500 . ?
C43D C44D 1.3900 . ?
C43D H43D 0.9500 . ?
C44D C45D 1.3900 . ?
C44D H44D 0.9500 . ?
C45D C46D 1.3900 . ?
C45D H45D 0.9500 . ?
C46D H46D 0.9500 . ?
C31D C32D 1.3900 . ?
C31D C36D 1.3900 . ?
C32D C33D 1.3900 . ?
C32D H32D 0.9500 . ?
C33D C34D 1.3900 . ?
C33D H33D 0.9500 . ?
C34D C35D 1.3900 . ?
C34D H34D 0.9500 . ?
C35D C36D 1.3900 . ?
C35D H35D 0.9500 . ?
C36D H36D 0.9500 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Rh1 N3' 85.13(15) . . ?
C2 Rh1 C1B 93.09(16) . . ?
N3' Rh1 C1B 152.70(16) . . ?
C2 Rh1 C2B 98.78(16) . . ?
N3' Rh1 C2B 169.66(15) . . ?
C1B Rh1 C2B 37.16(16) . . ?
C2 Rh1 C5B 162.54(16) . . ?
N3' Rh1 C5B 91.79(16) . . ?
C1B Rh1 C5B 97.37(18) . . ?
C2B Rh1 C5B 81.60(17) . . ?
C2 Rh1 C6B 160.07(16) . . ?
N3' Rh1 C6B 91.22(16) . . ?
C1B Rh1 C6B 81.23(17) . . ?
C2B Rh1 C6B 88.24(17) . . ?
C5B Rh1 C6B 36.83(17) . . ?
C2 N1 C5 111.2(3) . . ?
C2 N1 C6 126.3(3) . . ?
C5 N1 C6 122.5(3) . . ?
N3 C2 N1 103.3(3) . . ?
N3 C2 Rh1 122.1(3) . . ?
N1 C2 Rh1 134.4(3) . . ?
C2 N3 C4 112.4(3) . . ?
C2 N3 C1A 123.5(4) . . ?
C4 N3 C1A 124.1(4) . . ?
C5 C4 N3 106.5(4) . . ?
C5 C4 H4 126.7 . . ?
N3 C4 H4 126.7 . . ?
C4 C5 N1 106.6(4) . . ?
C4 C5 H5 126.7 . . ?
N1 C5 H5 126.7 . . ?
N3 C1A C4' 111.2(3) . . ?
N3 C1A H1A1 109.4 . . ?
C4' C1A H1A1 109.4 . . ?
N3 C1A H1A2 109.4 . . ?
C4' C1A H1A2 109.4 . . ?
H1A1 C1A H1A2 108.0 . . ?
N2' N1' C5' 111.7(4) . . ?
N2' N1' C6' 118.6(4) . . ?
C5' N1' C6' 129.4(4) . . ?
N3' N2' N1' 106.0(3) . . ?
N2' N3' C4' 109.0(4) . . ?
N2' N3' Rh1 127.2(3) . . ?
C4' N3' Rh1 123.6(3) . . ?
C5' C4' N3' 108.2(4) . . ?
C5' C4' C1A 131.7(4) . . ?
N3' C4' C1A 120.1(4) . . ?
N1' C5' C4' 105.0(4) . . ?
N1' C5' H5' 127.5 . . ?
C4' C5' H5' 127.5 . . ?
C7 C6 C11 123.3(4) . . ?
C7 C6 N1 118.7(4) . . ?
C11 C6 N1 118.0(4) . . ?
C6 C7 C8 115.7(5) . . ?
C6 C7 C12 122.4(4) . . ?
C8 C7 C12 121.9(4) . . ?
C9 C8 C7 123.4(5) . . ?
C9 C8 H8 118.3 . . ?
C7 C8 H8 118.3 . . ?
C8 C9 C10 118.2(5) . . ?
C8 C9 C13 120.9(5) . . ?
C10 C9 C13 120.9(6) . . ?
C9 C10 C11 122.2(5) . . ?
C9 C10 H6B 118.9 . . ?
C11 C10 H6B 118.9 . . ?
C6 C11 C10 117.2(4) . . ?
C6 C11 C14 122.0(4) . . ?
C10 C11 C14 120.8(4) . . ?
C7 C12 H12A 109.5 . . ?
C7 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C7 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C9 C13 H13A 109.5 . . ?
C9 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C9 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N1' C6' C7' 109.2(4) . . ?
N1' C6' H6'1 109.8 . . ?
C7' C6' H6'1 109.8 . . ?
N1' C6' H6'2 109.8 . . ?
C7' C6' H6'2 109.8 . . ?
H6'1 C6' H6'2 108.3 . . ?
C8' C7' C12' 118.9(5) . . ?
C8' C7' C6' 122.3(5) . . ?
C12' C7' C6' 118.8(4) . . ?
C7' C8' C9' 120.9(5) . . ?
C7' C8' H8' 119.5 . . ?
C9' C8' H8' 119.5 . . ?
C10' C9' C8' 116.8(5) . . ?
C10' C9' H9' 121.6 . . ?
C8' C9' H9' 121.6 . . ?
C9' C10' C11' 123.9(5) . . ?
C9' C10' N4' 116.7(5) . . ?
C11' C10' N4' 119.4(5) . . ?
C10' C11' C12' 117.7(5) . . ?
C10' C11' H11' 121.1 . . ?
C12' C11' H11' 121.1 . . ?
C11' C12' C7' 121.5(5) . . ?
C11' C12' H12' 119.3 . . ?
C7' C12' H12' 119.3 . . ?
O1' N4' O2' 124.6(6) . . ?
O1' N4' C10' 118.6(6) . . ?
O2' N4' C10' 116.8(6) . . ?
C2B C1B C8B 126.4(4) . . ?
C2B C1B Rh1 71.9(3) . . ?
C8B C1B Rh1 108.7(3) . . ?
C2B C1B H1B 116.8 . . ?
C8B C1B H1B 116.8 . . ?
Rh1 C1B H1B 89.4 . . ?
C1B C2B C3B 125.0(4) . . ?
C1B C2B Rh1 71.0(3) . . ?
C3B C2B Rh1 112.6(3) . . ?
C1B C2B H2B 117.5 . . ?
C3B C2B H2B 117.5 . . ?
Rh1 C2B H2B 86.4 . . ?
C2B C3B C4B 112.6(4) . . ?
C2B C3B H3B1 109.1 . . ?
C4B C3B H3B1 109.1 . . ?
C2B C3B H3B2 109.1 . . ?
C4B C3B H3B2 109.1 . . ?
H3B1 C3B H3B2 107.8 . . ?
C5B C4B C3B 113.7(4) . . ?
C5B C4B H4B1 108.8 . . ?
C3B C4B H4B1 108.8 . . ?
C5B C4B H4B2 108.8 . . ?
C3B C4B H4B2 108.8 . . ?
H4B1 C4B H4B2 107.7 . . ?
C6B C5B C4B 125.0(5) . . ?
C6B C5B Rh1 72.1(2) . . ?
C4B C5B Rh1 108.0(3) . . ?
C6B C5B H5B 117.5 . . ?
C4B C5B H5B 117.5 . . ?
Rh1 C5B H5B 89.9 . . ?
C5B C6B C7B 124.6(4) . . ?
C5B C6B Rh1 71.1(2) . . ?
C7B C6B Rh1 111.3(3) . . ?
C5B C6B H6B1 117.7 . . ?
C7B C6B H6B1 117.7 . . ?
Rh1 C6B H6B1 87.5 . . ?
C6B C7B C8B 112.4(4) . . ?
C6B C7B H7B1 109.1 . . ?
C8B C7B H7B1 109.1 . . ?
C6B C7B H7B2 109.1 . . ?
C8B C7B H7B2 109.1 . . ?
H7B1 C7B H7B2 107.9 . . ?
C1B C8B C7B 112.9(4) . . ?
C1B C8B H8B1 109.0 . . ?
C7B C8B H8B1 109.0 . . ?
C1B C8B H8B2 109.0 . . ?
C7B C8B H8B2 109.0 . . ?
H8B1 C8B H8B2 107.8 . . ?
C21D B1D C11D 109.3(3) . . ?
C21D B1D C41D 109.6(3) . . ?
C11D B1D C41D 109.0(3) . . ?
C21D B1D C31D 108.6(3) . . ?
C11D B1D C31D 107.4(3) . . ?
C41D B1D C31D 112.8(3) . . ?
C12D C11D C16D 115.2(4) . . ?
C12D C11D B1D 121.7(4) . . ?
C16D C11D B1D 123.0(4) . . ?
C13D C12D C11D 122.9(4) . . ?
C13D C12D H12D 118.6 . . ?
C11D C12D H12D 118.6 . . ?
C14D C13D C12D 119.6(4) . . ?
C14D C13D H13D 120.2 . . ?
C12D C13D H13D 120.2 . . ?
C15D C14D C13D 119.6(4) . . ?
C15D C14D H14D 120.2 . . ?
C13D C14D H14D 120.2 . . ?
C14D C15D C16D 119.7(4) . . ?
C14D C15D H15D 120.1 . . ?
C16D C15D H15D 120.1 . . ?
C15D C16D C11D 122.9(4) . . ?
C15D C16D H16D 118.5 . . ?
C11D C16D H16D 118.5 . . ?
C22D C21D C26D 115.0(4) . . ?
C22D C21D B1D 122.9(4) . . ?
C26D C21D B1D 122.1(4) . . ?
C23D C22D C21D 123.4(5) . . ?
C23D C22D H22D 118.3 . . ?
C21D C22D H22D 118.3 . . ?
C24D C23D C22D 119.8(5) . . ?
C24D C23D H23D 120.1 . . ?
C22D C23D H23D 120.1 . . ?
C23D C24D C25D 119.2(4) . . ?
C23D C24D H24D 120.4 . . ?
C25D C24D H24D 120.4 . . ?
C24D C25D C26D 119.9(5) . . ?
C24D C25D H25D 120.0 . . ?
C26D C25D H25D 120.0 . . ?
C25D C26D C21D 122.6(4) . . ?
C25D C26D H26D 118.7 . . ?
C21D C26D H26D 118.7 . . ?
C42D C41D C46D 120.0 . . ?
C42D C41D B1D 121.2(3) . . ?
C46D C41D B1D 118.8(3) . . ?
C43D C42D C41D 120.0 . . ?
C43D C42D H42D 120.0 . . ?
C41D C42D H42D 120.0 . . ?
C42D C43D C44D 120.0 . . ?
C42D C43D H43D 120.0 . . ?
C44D C43D H43D 120.0 . . ?
C45D C44D C43D 120.0 . . ?
C45D C44D H44D 120.0 . . ?
C43D C44D H44D 120.0 . . ?
C44D C45D C46D 120.0 . . ?
C44D C45D H45D 120.0 . . ?
C46D C45D H45D 120.0 . . ?
C45D C46D C41D 120.0 . . ?
C45D C46D H46D 120.0 . . ?
C41D C46D H46D 120.0 . . ?
C32D C31D C36D 120.0 . . ?
C32D C31D B1D 119.1(2) . . ?
C36D C31D B1D 120.9(2) . . ?
C31D C32D C33D 120.0 . . ?
C31D C32D H32D 120.0 . . ?
C33D C32D H32D 120.0 . . ?
C34D C33D C32D 120.0 . . ?
C34D C33D H33D 120.0 . . ?
C32D C33D H33D 120.0 . . ?
C33D C34D C35D 120.0 . . ?
C33D C34D H34D 120.0 . . ?
C35D C34D H34D 120.0 . . ?
C36D C35D C34D 120.0 . . ?
C36D C35D H35D 120.0 . . ?
C34D C35D H35D 120.0 . . ?
C35D C36D C31D 120.0 . . ?
C35D C36D H36D 120.0 . . ?
C31D C36D H36D 120.0 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 C2 N3 0.5(4) . . . . ?
C6 N1 C2 N3 177.6(3) . . . . ?
C5 N1 C2 Rh1 -174.1(3) . . . . ?
C6 N1 C2 Rh1 3.0(6) . . . . ?
N3' Rh1 C2 N3 -33.8(3) . . . . ?
C1B Rh1 C2 N3 118.9(3) . . . . ?
C2B Rh1 C2 N3 155.8(3) . . . . ?
C5B Rh1 C2 N3 -114.3(6) . . . . ?
C6B Rh1 C2 N3 46.2(7) . . . . ?
N3' Rh1 C2 N1 139.9(4) . . . . ?
C1B Rh1 C2 N1 -67.4(4) . . . . ?
C2B Rh1 C2 N1 -30.4(4) . . . . ?
C5B Rh1 C2 N1 59.5(8) . . . . ?
C6B Rh1 C2 N1 -140.0(5) . . . . ?
N1 C2 N3 C4 -0.1(4) . . . . ?
Rh1 C2 N3 C4 175.3(3) . . . . ?
N1 C2 N3 C1A 179.8(4) . . . . ?
Rh1 C2 N3 C1A -4.7(5) . . . . ?
C2 N3 C4 C5 -0.3(5) . . . . ?
C1A N3 C4 C5 179.7(4) . . . . ?
N3 C4 C5 N1 0.6(5) . . . . ?
C2 N1 C5 C4 -0.7(5) . . . . ?
C6 N1 C5 C4 -178.0(4) . . . . ?
C2 N3 C1A C4' 54.1(6) . . . . ?
C4 N3 C1A C4' -126.0(4) . . . . ?
C5' N1' N2' N3' 0.0(5) . . . . ?
C6' N1' N2' N3' 174.8(4) . . . . ?
N1' N2' N3' C4' -0.1(4) . . . . ?
N1' N2' N3' Rh1 -174.1(3) . . . . ?
C2 Rh1 N3' N2' -148.2(3) . . . . ?
C1B Rh1 N3' N2' 124.5(4) . . . . ?
C2B Rh1 N3' N2' -35.4(10) . . . . ?
C5B Rh1 N3' N2' 14.6(3) . . . . ?
C6B Rh1 N3' N2' 51.4(3) . . . . ?
C2 Rh1 N3' C4' 38.6(3) . . . . ?
C1B Rh1 N3' C4' -48.7(5) . . . . ?
C2B Rh1 N3' C4' 151.4(7) . . . . ?
C5B Rh1 N3' C4' -158.6(3) . . . . ?
C6B Rh1 N3' C4' -121.8(3) . . . . ?
N2' N3' C4' C5' 0.1(5) . . . . ?
Rh1 N3' C4' C5' 174.4(3) . . . . ?
N2' N3' C4' C1A -178.5(4) . . . . ?
Rh1 N3' C4' C1A -4.2(6) . . . . ?
N3 C1A C4' C5' 134.1(5) . . . . ?
N3 C1A C4' N3' -47.7(6) . . . . ?
N2' N1' C5' C4' 0.1(5) . . . . ?
C6' N1' C5' C4' -174.0(4) . . . . ?
N3' C4' C5' N1' -0.1(5) . . . . ?
C1A C4' C5' N1' 178.2(5) . . . . ?
C2 N1 C6 C7 105.9(5) . . . . ?
C5 N1 C6 C7 -77.3(5) . . . . ?
C2 N1 C6 C11 -76.2(5) . . . . ?
C5 N1 C6 C11 100.6(5) . . . . ?
C11 C6 C7 C8 -0.2(6) . . . . ?
N1 C6 C7 C8 177.6(3) . . . . ?
C11 C6 C7 C12 -178.9(4) . . . . ?
N1 C6 C7 C12 -1.1(6) . . . . ?
C6 C7 C8 C9 0.2(6) . . . . ?
C12 C7 C8 C9 178.9(4) . . . . ?
C7 C8 C9 C10 1.0(7) . . . . ?
C7 C8 C9 C13 -178.1(4) . . . . ?
C8 C9 C10 C11 -2.2(7) . . . . ?
C13 C9 C10 C11 176.9(4) . . . . ?
C7 C6 C11 C10 -0.9(6) . . . . ?
N1 C6 C11 C10 -178.7(3) . . . . ?
C7 C6 C11 C14 -179.9(4) . . . . ?
N1 C6 C11 C14 2.3(6) . . . . ?
C9 C10 C11 C6 2.1(6) . . . . ?
C9 C10 C11 C14 -178.8(4) . . . . ?
N2' N1' C6' C7' -69.6(5) . . . . ?
C5' N1' C6' C7' 104.1(5) . . . . ?
N1' C6' C7' C8' -85.0(6) . . . . ?
N1' C6' C7' C12' 93.7(5) . . . . ?
C12' C7' C8' C9' -5.2(8) . . . . ?
C6' C7' C8' C9' 173.5(5) . . . . ?
C7' C8' C9' C10' 1.9(8) . . . . ?
C8' C9' C10' C11' 3.8(8) . . . . ?
C8' C9' C10' N4' -177.8(5) . . . . ?
C9' C10' C11' C12' -5.7(9) . . . . ?
N4' C10' C11' C12' 176.0(5) . . . . ?
C10' C11' C12' C7' 2.0(9) . . . . ?
C8' C7' C12' C11' 3.3(9) . . . . ?
C6' C7' C12' C11' -175.5(5) . . . . ?
C9' C10' N4' O1' 14.5(7) . . . . ?
C11' C10' N4' O1' -167.0(6) . . . . ?
C9' C10' N4' O2' -165.7(5) . . . . ?
C11' C10' N4' O2' 12.8(8) . . . . ?
C2 Rh1 C1B C2B 100.5(3) . . . . ?
N3' Rh1 C1B C2B -174.1(3) . . . . ?
C5B Rh1 C1B C2B -65.5(3) . . . . ?
C6B Rh1 C1B C2B -98.7(3) . . . . ?
C2 Rh1 C1B C8B -136.3(3) . . . . ?
N3' Rh1 C1B C8B -50.9(5) . . . . ?
C2B Rh1 C1B C8B 123.2(4) . . . . ?
C5B Rh1 C1B C8B 57.7(3) . . . . ?
C6B Rh1 C1B C8B 24.5(3) . . . . ?
C8B C1B C2B C3B 4.5(7) . . . . ?
Rh1 C1B C2B C3B 104.7(4) . . . . ?
C8B C1B C2B Rh1 -100.2(5) . . . . ?
C2 Rh1 C2B C1B -83.5(3) . . . . ?
N3' Rh1 C2B C1B 164.9(7) . . . . ?
C5B Rh1 C2B C1B 114.2(3) . . . . ?
C6B Rh1 C2B C1B 77.8(3) . . . . ?
C2 Rh1 C2B C3B 155.6(3) . . . . ?
N3' Rh1 C2B C3B 43.9(10) . . . . ?
C1B Rh1 C2B C3B -120.9(4) . . . . ?
C5B Rh1 C2B C3B -6.8(3) . . . . ?
C6B Rh1 C2B C3B -43.2(3) . . . . ?
C1B C2B C3B C4B -93.4(5) . . . . ?
Rh1 C2B C3B C4B -11.4(5) . . . . ?
C2B C3B C4B C5B 33.0(6) . . . . ?
C3B C4B C5B C6B 43.1(6) . . . . ?
C3B C4B C5B Rh1 -37.3(5) . . . . ?
C2 Rh1 C5B C6B 169.1(5) . . . . ?
N3' Rh1 C5B C6B 89.6(3) . . . . ?
C1B Rh1 C5B C6B -64.6(3) . . . . ?
C2B Rh1 C5B C6B -98.4(3) . . . . ?
C2 Rh1 C5B C4B -69.0(7) . . . . ?
N3' Rh1 C5B C4B -148.4(3) . . . . ?
C1B Rh1 C5B C4B 57.4(3) . . . . ?
C2B Rh1 C5B C4B 23.6(3) . . . . ?
C6B Rh1 C5B C4B 122.0(5) . . . . ?
C4B C5B C6B C7B 3.6(7) . . . . ?
Rh1 C5B C6B C7B 103.4(4) . . . . ?
C4B C5B C6B Rh1 -99.8(4) . . . . ?
C2 Rh1 C6B C5B -170.4(4) . . . . ?
N3' Rh1 C6B C5B -91.4(3) . . . . ?
C1B Rh1 C6B C5B 115.0(3) . . . . ?
C2B Rh1 C6B C5B 78.3(3) . . . . ?
C2 Rh1 C6B C7B 68.9(6) . . . . ?
N3' Rh1 C6B C7B 148.0(3) . . . . ?
C1B Rh1 C6B C7B -5.7(3) . . . . ?
C2B Rh1 C6B C7B -42.4(3) . . . . ?
C5B Rh1 C6B C7B -120.7(5) . . . . ?
C5B C6B C7B C8B -95.5(5) . . . . ?
Rh1 C6B C7B C8B -14.3(5) . . . . ?
C2B C1B C8B C7B 40.6(7) . . . . ?
Rh1 C1B C8B C7B -40.2(5) . . . . ?
C6B C7B C8B C1B 36.5(6) . . . . ?
C21D B1D C11D C12D -164.7(4) . . . . ?
C41D B1D C11D C12D -44.9(5) . . . . ?
C31D B1D C11D C12D 77.6(4) . . . . ?
C21D B1D C11D C16D 20.0(5) . . . . ?
C41D B1D C11D C16D 139.8(4) . . . . ?
C31D B1D C11D C16D -97.7(4) . . . . ?
C16D C11D C12D C13D -1.2(6) . . . . ?
B1D C11D C12D C13D -176.9(4) . . . . ?
C11D C12D C13D C14D -0.3(7) . . . . ?
C12D C13D C14D C15D 1.9(7) . . . . ?
C13D C14D C15D C16D -1.9(7) . . . . ?
C14D C15D C16D C11D 0.4(7) . . . . ?
C12D C11D C16D C15D 1.2(6) . . . . ?
B1D C11D C16D C15D 176.8(4) . . . . ?
C11D B1D C21D C22D 97.0(4) . . . . ?
C41D B1D C21D C22D -22.5(5) . . . . ?
C31D B1D C21D C22D -146.1(4) . . . . ?
C11D B1D C21D C26D -81.2(4) . . . . ?
C41D B1D C21D C26D 159.3(3) . . . . ?
C31D B1D C21D C26D 35.8(5) . . . . ?
C26D C21D C22D C23D -0.4(6) . . . . ?
B1D C21D C22D C23D -178.7(4) . . . . ?
C21D C22D C23D C24D 1.4(7) . . . . ?
C22D C23D C24D C25D -0.5(7) . . . . ?
C23D C24D C25D C26D -1.3(7) . . . . ?
C24D C25D C26D C21D 2.4(6) . . . . ?
C22D C21D C26D C25D -1.5(6) . . . . ?
B1D C21D C26D C25D 176.8(4) . . . . ?
C21D B1D C41D C42D -93.2(3) . . . . ?
C11D B1D C41D C42D 147.2(3) . . . . ?
C31D B1D C41D C42D 27.9(4) . . . . ?
C21D B1D C41D C46D 87.7(3) . . . . ?
C11D B1D C41D C46D -32.0(4) . . . . ?
C31D B1D C41D C46D -151.2(2) . . . . ?
C46D C41D C42D C43D 0.0 . . . . ?
B1D C41D C42D C43D -179.1(3) . . . . ?
C41D C42D C43D C44D 0.0 . . . . ?
C42D C43D C44D C45D 0.0 . . . . ?
C43D C44D C45D C46D 0.0 . . . . ?
C44D C45D C46D C41D 0.0 . . . . ?
C42D C41D C46D C45D 0.0 . . . . ?
B1D C41D C46D C45D 179.1(3) . . . . ?
C21D B1D C31D C32D 52.0(4) . . . . ?
C11D B1D C31D C32D 170.2(3) . . . . ?
C41D B1D C31D C32D -69.7(4) . . . . ?
C21D B1D C31D C36D -129.6(3) . . . . ?
C11D B1D C31D C36D -11.5(4) . . . . ?
C41D B1D C31D C36D 108.7(3) . . . . ?
C36D C31D C32D C33D 0.0 . . . . ?
B1D C31D C32D C33D 178.4(3) . . . . ?
C31D C32D C33D C34D 0.0 . . . . ?
C32D C33D C34D C35D 0.0 . . . . ?
C33D C34D C35D C36D 0.0 . . . . ?
C34D C35D C36D C31D 0.0 . . . . ?
C32D C31D C36D C35D 0.0 . . . . ?
B1D C31D C36D C35D -178.3(3) . . . . ?
_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max 1.409
_refine_diff_density_min -0.613
_refine_diff_density_rms 0.077
_database_code_depnum_ccdc_archive 'CCDC 934037'
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_inp1bar3
#TrackingRef 'Khuong5_Deposition_18May12.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C31 H37 N5 O Rh, C24 H20 B'
_chemical_formula_sum 'C55 H57 B N5 O Rh'
_chemical_formula_weight 917.78
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Triclinic
_symmetry_space_group_name_H-M P-1
_symmetry_space_group_name_Hall '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 11.0626(7)
_cell_length_b 15.0649(4)
_cell_length_c 15.9240(3)
_cell_angle_alpha 114.2700(10)
_cell_angle_beta 99.4070(10)
_cell_angle_gamma 98.5590(10)
_cell_volume 2316.89(16)
_cell_formula_units_Z 2
_cell_measurement_temperature 150(2)
_cell_measurement_reflns_used 9855
_cell_measurement_theta_min 2.150
_cell_measurement_theta_max 30.28
_exptl_crystal_description Plates
_exptl_crystal_colour Yellow
_exptl_crystal_size_max 0.32
_exptl_crystal_size_mid 0.22
_exptl_crystal_size_min 0.12
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.316
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 960
_exptl_absorpt_coefficient_mu 0.414
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.8800
_exptl_absorpt_correction_T_max 0.9501
_exptl_absorpt_process_details 'SADABS (Bruker, 2001)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 150(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker kappa APEXII CCD Diffractometer'
_diffrn_measurement_method '\f scans, and \w scans with \k offsets'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 28873
_diffrn_reflns_av_R_equivalents 0.0515
_diffrn_reflns_av_sigmaI/netI 0.0426
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_theta_min 2.53
_diffrn_reflns_theta_max 25.00
_reflns_number_total 8046
_reflns_number_gt 7337
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2007)'
_computing_cell_refinement 'APEX2 (Bruker, 2007)'
_computing_data_reduction 'APEX2 (Bruker, 2007)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0080P)^2^+1.4798P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 8046
_refine_ls_number_parameters 572
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0311
_refine_ls_R_factor_gt 0.0271
_refine_ls_wR_factor_ref 0.0695
_refine_ls_wR_factor_gt 0.0665
_refine_ls_goodness_of_fit_ref 1.070
_refine_ls_restrained_S_all 1.070
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.738419(14) 0.628377(11) 0.692072(10) 0.01939(6) Uani 1 1 d . . .
N1 N 0.78445(15) 0.78600(12) 0.90544(11) 0.0199(3) Uani 1 1 d . . .
C2 C 0.73044(18) 0.75013(14) 0.81111(14) 0.0202(4) Uani 1 1 d . . .
N3 N 0.68185(15) 0.82595(12) 0.80651(11) 0.0214(3) Uani 1 1 d . . .
C4 C 0.70481(19) 0.90676(15) 0.89535(14) 0.0242(4) Uani 1 1 d . . .
H4 H 0.6796 0.9679 0.9094 0.029 Uiso 1 1 calc R . .
C5 C 0.76945(19) 0.88156(15) 0.95739(14) 0.0244(4) Uani 1 1 d . . .
H5 H 0.7993 0.9215 1.0242 0.029 Uiso 1 1 calc R . .
C1A C 0.6193(2) 0.82342(16) 0.71703(14) 0.0264(4) Uani 1 1 d . . .
H1A1 H 0.5970 0.8882 0.7299 0.032 Uiso 1 1 calc R . .
H1A2 H 0.5403 0.7699 0.6875 0.032 Uiso 1 1 calc R . .
N1' N 0.80990(16) 0.79864(12) 0.54792(12) 0.0243(4) Uani 1 1 d . . .
N2' N 0.82879(15) 0.72523(12) 0.57057(12) 0.0235(4) Uani 1 1 d . . .
N3' N 0.76259(15) 0.72916(12) 0.63355(11) 0.0213(3) Uani 1 1 d . . .
C4' C 0.70274(19) 0.80444(14) 0.65006(14) 0.0227(4) Uani 1 1 d . . .
C5' C 0.73237(19) 0.84942(15) 0.59492(14) 0.0258(4) Uani 1 1 d . . .
H5' H 0.7045 0.9044 0.5906 0.031 Uiso 1 1 calc R . .
C6 C 0.84762(18) 0.73425(14) 0.95100(13) 0.0211(4) Uani 1 1 d . . .
C7 C 0.7838(2) 0.69730(15) 1.00298(14) 0.0258(4) Uani 1 1 d . . .
C8 C 0.8492(2) 0.65431(16) 1.05234(15) 0.0332(5) Uani 1 1 d . . .
H8 H 0.8081 0.6289 1.0886 0.040 Uiso 1 1 calc R . .
C9 C 0.9715(2) 0.64744(16) 1.05036(15) 0.0354(5) Uani 1 1 d . . .
C10 C 1.0297(2) 0.68160(16) 0.99466(16) 0.0348(5) Uani 1 1 d . . .
H10 H 1.1127 0.6741 0.9907 0.042 Uiso 1 1 calc R . .
C11 C 0.96989(19) 0.72645(15) 0.94451(14) 0.0262(4) Uani 1 1 d . . .
C12 C 0.6512(2) 0.70431(18) 1.00791(17) 0.0363(5) Uani 1 1 d . . .
H12A H 0.6097 0.6490 1.0185 0.054 Uiso 1 1 calc R . .
H12B H 0.6046 0.7001 0.9480 0.054 Uiso 1 1 calc R . .
H12C H 0.6525 0.7684 1.0605 0.054 Uiso 1 1 calc R . .
C13 C 1.0431(3) 0.6085(2) 1.1120(2) 0.0562(8) Uani 1 1 d . . .
H13G H 1.0898 0.6648 1.1731 0.084 Uiso 1 1 calc R . .
H13E H 1.1024 0.5736 1.0798 0.084 Uiso 1 1 calc R . .
H13F H 0.9834 0.5618 1.1229 0.084 Uiso 1 1 calc R . .
C14 C 1.0353(2) 0.76536(19) 0.88645(18) 0.0372(5) Uani 1 1 d . . .
H14A H 0.9843 0.7336 0.8206 0.056 Uiso 1 1 calc R . .
H14B H 1.1183 0.7497 0.8879 0.056 Uiso 1 1 calc R . .
H14C H 1.0460 0.8382 0.9131 0.056 Uiso 1 1 calc R . .
C6' C 0.8618(2) 0.80894(17) 0.47196(15) 0.0311(5) Uani 1 1 d . . .
H6'1 H 0.9427 0.7883 0.4723 0.037 Uiso 1 1 calc R . .
H6'2 H 0.8789 0.8801 0.4841 0.037 Uiso 1 1 calc R . .
C7' C 0.7714(2) 0.74557(15) 0.37640(15) 0.0264(4) Uani 1 1 d . . .
C8' C 0.7811(2) 0.64971(17) 0.31879(16) 0.0334(5) Uani 1 1 d . . .
H8' H 0.8489 0.6251 0.3387 0.040 Uiso 1 1 calc R . .
C9' C 0.6942(2) 0.58973(17) 0.23339(16) 0.0348(5) Uani 1 1 d . . .
H9' H 0.7024 0.5244 0.1949 0.042 Uiso 1 1 calc R . .
C10' C 0.5944(2) 0.62478(16) 0.20345(15) 0.0292(5) Uani 1 1 d . . .
C11' C 0.5839(2) 0.72068(16) 0.25904(15) 0.0288(5) Uani 1 1 d . . .
H11' H 0.5166 0.7455 0.2386 0.035 Uiso 1 1 calc R . .
C12' C 0.6722(2) 0.78019(15) 0.34470(15) 0.0274(5) Uani 1 1 d . . .
H12' H 0.6649 0.8460 0.3826 0.033 Uiso 1 1 calc R . .
C13' C 0.4014(2) 0.5877(2) 0.09085(18) 0.0458(6) Uani 1 1 d . . .
H13A H 0.3537 0.5986 0.1395 0.069 Uiso 1 1 calc R . .
H13B H 0.3494 0.5341 0.0298 0.069 Uiso 1 1 calc R . .
H13C H 0.4240 0.6497 0.0846 0.069 Uiso 1 1 calc R . .
O1' O 0.51302(16) 0.55971(11) 0.11784(11) 0.0394(4) Uani 1 1 d . . .
C5B C 0.6952(2) 0.50255(15) 0.54853(14) 0.0267(5) Uani 1 1 d . . .
H5B H 0.6694 0.5461 0.5235 0.032 Uiso 1 1 calc R . .
C6B C 0.8212(2) 0.52366(16) 0.59137(15) 0.0293(5) Uani 1 1 d . . .
H6B H 0.8748 0.5795 0.5920 0.035 Uiso 1 1 calc R . .
C7B C 0.8820(2) 0.46646(18) 0.63733(17) 0.0402(6) Uani 1 1 d . . .
H71B H 0.9670 0.5074 0.6775 0.048 Uiso 1 1 calc R . .
H72B H 0.8925 0.4040 0.5872 0.048 Uiso 1 1 calc R . .
C8B C 0.8048(3) 0.43972(17) 0.69840(17) 0.0409(6) Uani 1 1 d . . .
H82B H 0.7400 0.3765 0.6574 0.049 Uiso 1 1 calc R . .
H81B H 0.8611 0.4281 0.7460 0.049 Uiso 1 1 calc R . .
C1B C 0.7402(2) 0.52079(15) 0.74971(15) 0.0308(5) Uani 1 1 d . . .
H1B H 0.7871 0.5745 0.8090 0.037 Uiso 1 1 calc R . .
C2B C 0.6166(2) 0.52143(16) 0.71542(15) 0.0304(5) Uani 1 1 d . . .
H2B H 0.5837 0.5743 0.7541 0.036 Uiso 1 1 calc R . .
C3B C 0.5309(2) 0.44430(18) 0.62125(16) 0.0394(6) Uani 1 1 d . . .
H31B H 0.4572 0.4702 0.6065 0.047 Uiso 1 1 calc R . .
H32B H 0.4992 0.3828 0.6273 0.047 Uiso 1 1 calc R . .
C4B C 0.5935(2) 0.41628(16) 0.53747(15) 0.0342(5) Uani 1 1 d . . .
H41B H 0.6312 0.3591 0.5320 0.041 Uiso 1 1 calc R . .
H42B H 0.5281 0.3943 0.4779 0.041 Uiso 1 1 calc R . .
B1D B 0.2829(2) 0.92888(16) 0.70386(15) 0.0202(4) Uani 1 1 d . . .
C11D C 0.41193(18) 1.01084(14) 0.77998(13) 0.0198(4) Uani 1 1 d . . .
C12D C 0.42657(19) 1.03915(15) 0.87743(14) 0.0253(4) Uani 1 1 d . . .
H12D H 0.3608 1.0102 0.8967 0.030 Uiso 1 1 calc R . .
C13D C 0.5316(2) 1.10700(15) 0.94701(15) 0.0292(5) Uani 1 1 d . . .
H13D H 0.5372 1.1232 1.0120 0.035 Uiso 1 1 calc R . .
C14D C 0.6282(2) 1.15081(16) 0.92121(16) 0.0335(5) Uani 1 1 d . . .
H14D H 0.7008 1.1973 0.9682 0.040 Uiso 1 1 calc R . .
C15D C 0.6181(2) 1.12644(16) 0.82665(17) 0.0328(5) Uani 1 1 d . . .
H15D H 0.6842 1.1566 0.8085 0.039 Uiso 1 1 calc R . .
C16D C 0.51168(19) 1.05783(15) 0.75702(15) 0.0244(4) Uani 1 1 d . . .
H16D H 0.5068 1.0426 0.6923 0.029 Uiso 1 1 calc R . .
C21D C 0.27779(18) 0.91239(14) 0.59460(13) 0.0216(4) Uani 1 1 d . . .
C22D C 0.3668(2) 0.86977(17) 0.54778(15) 0.0317(5) Uani 1 1 d . . .
H22D H 0.4309 0.8525 0.5813 0.038 Uiso 1 1 calc R . .
C23D C 0.3654(3) 0.85179(19) 0.45511(17) 0.0427(6) Uani 1 1 d . . .
H23D H 0.4285 0.8237 0.4269 0.051 Uiso 1 1 calc R . .
C24D C 0.2728(3) 0.87452(19) 0.40366(17) 0.0467(7) Uani 1 1 d . . .
H24D H 0.2716 0.8626 0.3401 0.056 Uiso 1 1 calc R . .
C25D C 0.1818(2) 0.91494(17) 0.44594(16) 0.0390(6) Uani 1 1 d . . .
H25D H 0.1164 0.9299 0.4110 0.047 Uiso 1 1 calc R . .
C26D C 0.1855(2) 0.93384(15) 0.53943(15) 0.0272(4) Uani 1 1 d . . .
H26D H 0.1225 0.9626 0.5672 0.033 Uiso 1 1 calc R . .
C31D C 0.16369(18) 0.97247(14) 0.74089(13) 0.0202(4) Uani 1 1 d . . .
C32D C 0.1476(2) 1.06577(16) 0.74774(15) 0.0286(5) Uani 1 1 d . . .
H32D H 0.2068 1.1032 0.7302 0.034 Uiso 1 1 calc R . .
C33D C 0.0493(2) 1.10544(17) 0.77891(16) 0.0365(5) Uani 1 1 d . . .
H33D H 0.0401 1.1676 0.7800 0.044 Uiso 1 1 calc R . .
C34D C -0.0357(2) 1.05471(18) 0.80855(16) 0.0394(6) Uani 1 1 d . . .
H34D H -0.1027 1.0819 0.8309 0.047 Uiso 1 1 calc R . .
C35D C -0.0213(2) 0.96451(18) 0.80500(16) 0.0351(5) Uani 1 1 d . . .
H35D H -0.0779 0.9297 0.8264 0.042 Uiso 1 1 calc R . .
C36D C 0.07499(19) 0.92354(16) 0.77043(14) 0.0259(4) Uani 1 1 d . . .
H36D H 0.0807 0.8598 0.7667 0.031 Uiso 1 1 calc R . .
C41D C 0.27496(18) 0.81836(14) 0.70373(13) 0.0202(4) Uani 1 1 d . . .
C42D C 0.1835(2) 0.73430(15) 0.63255(14) 0.0261(4) Uani 1 1 d . . .
H42D H 0.1294 0.7426 0.5849 0.031 Uiso 1 1 calc R . .
C43D C 0.1689(2) 0.63979(16) 0.62909(16) 0.0317(5) Uani 1 1 d . . .
H43D H 0.1054 0.5852 0.5799 0.038 Uiso 1 1 calc R . .
C44D C 0.2466(2) 0.62473(16) 0.69683(17) 0.0363(5) Uani 1 1 d . . .
H44D H 0.2377 0.5598 0.6941 0.044 Uiso 1 1 calc R . .
C45D C 0.3370(2) 0.70520(17) 0.76841(17) 0.0364(5) Uani 1 1 d . . .
H45D H 0.3907 0.6961 0.8157 0.044 Uiso 1 1 calc R . .
C46D C 0.3496(2) 0.79967(16) 0.77136(15) 0.0271(4) Uani 1 1 d . . .
H46D H 0.4120 0.8541 0.8218 0.033 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Rh1 0.02415(10) 0.01826(9) 0.01732(9) 0.00988(7) 0.00298(6) 0.00613(6)
N1 0.0213(9) 0.0217(8) 0.0184(8) 0.0101(7) 0.0051(6) 0.0063(7)
C2 0.0181(10) 0.0219(10) 0.0239(10) 0.0134(8) 0.0052(8) 0.0047(8)
N3 0.0223(9) 0.0235(9) 0.0215(8) 0.0118(7) 0.0061(7) 0.0091(7)
C4 0.0265(11) 0.0227(10) 0.0268(11) 0.0106(9) 0.0125(9) 0.0104(9)
C5 0.0283(11) 0.0225(10) 0.0221(10) 0.0081(8) 0.0094(8) 0.0072(9)
C1A 0.0278(11) 0.0331(12) 0.0259(11) 0.0178(9) 0.0060(9) 0.0155(9)
N1' 0.0260(9) 0.0257(9) 0.0243(9) 0.0163(7) 0.0037(7) 0.0029(7)
N2' 0.0236(9) 0.0259(9) 0.0238(9) 0.0143(7) 0.0053(7) 0.0048(7)
N3' 0.0224(9) 0.0233(9) 0.0203(8) 0.0116(7) 0.0048(7) 0.0062(7)
C4' 0.0235(10) 0.0232(10) 0.0221(10) 0.0127(8) 0.0010(8) 0.0054(9)
C5' 0.0284(11) 0.0240(11) 0.0275(11) 0.0150(9) 0.0029(9) 0.0071(9)
C6 0.0254(11) 0.0185(10) 0.0160(9) 0.0070(8) -0.0007(8) 0.0039(8)
C7 0.0350(12) 0.0206(10) 0.0178(10) 0.0070(8) 0.0035(8) 0.0034(9)
C8 0.0496(15) 0.0255(11) 0.0224(11) 0.0130(9) 0.0025(10) 0.0029(10)
C9 0.0476(15) 0.0241(11) 0.0273(11) 0.0121(9) -0.0082(10) 0.0060(10)
C10 0.0287(12) 0.0293(12) 0.0386(13) 0.0130(10) -0.0043(10) 0.0055(10)
C11 0.0261(11) 0.0226(11) 0.0250(10) 0.0093(9) -0.0004(8) 0.0039(9)
C12 0.0411(14) 0.0394(13) 0.0395(13) 0.0241(11) 0.0200(11) 0.0112(11)
C13 0.0660(19) 0.0472(16) 0.0522(17) 0.0302(14) -0.0138(14) 0.0118(14)
C14 0.0240(12) 0.0486(15) 0.0466(14) 0.0274(12) 0.0107(10) 0.0099(11)
C6' 0.0299(12) 0.0365(13) 0.0330(12) 0.0230(10) 0.0095(9) 0.0018(10)
C7' 0.0287(11) 0.0304(11) 0.0286(11) 0.0206(9) 0.0123(9) 0.0041(9)
C8' 0.0387(13) 0.0383(13) 0.0371(13) 0.0252(11) 0.0151(10) 0.0174(11)
C9' 0.0514(15) 0.0284(12) 0.0317(12) 0.0156(10) 0.0152(11) 0.0177(11)
C10' 0.0379(13) 0.0277(11) 0.0258(11) 0.0157(9) 0.0112(9) 0.0035(10)
C11' 0.0322(12) 0.0286(11) 0.0324(12) 0.0187(10) 0.0102(9) 0.0089(10)
C12' 0.0343(12) 0.0222(11) 0.0297(11) 0.0146(9) 0.0115(9) 0.0055(9)
C13' 0.0385(14) 0.0471(15) 0.0402(14) 0.0157(12) -0.0008(11) 0.0004(12)
O1' 0.0494(10) 0.0322(9) 0.0297(9) 0.0113(7) 0.0027(7) 0.0056(8)
C5B 0.0380(13) 0.0226(11) 0.0184(10) 0.0081(8) 0.0036(9) 0.0109(9)
C6B 0.0385(13) 0.0236(11) 0.0260(11) 0.0083(9) 0.0090(9) 0.0154(10)
C7B 0.0473(15) 0.0359(13) 0.0370(13) 0.0138(11) 0.0032(11) 0.0240(12)
C8B 0.0601(16) 0.0271(12) 0.0331(13) 0.0156(10) -0.0058(11) 0.0159(11)
C1B 0.0488(14) 0.0195(11) 0.0220(10) 0.0127(9) -0.0009(9) 0.0028(10)
C2B 0.0419(13) 0.0237(11) 0.0292(11) 0.0169(9) 0.0086(10) 0.0032(10)
C3B 0.0406(14) 0.0384(13) 0.0362(13) 0.0228(11) -0.0005(10) -0.0063(11)
C4B 0.0425(14) 0.0251(11) 0.0252(11) 0.0092(9) -0.0048(10) 0.0009(10)
B1D 0.0198(11) 0.0226(11) 0.0196(11) 0.0098(9) 0.0064(9) 0.0060(9)
C11D 0.0191(10) 0.0186(10) 0.0236(10) 0.0094(8) 0.0066(8) 0.0083(8)
C12D 0.0226(11) 0.0275(11) 0.0249(10) 0.0093(9) 0.0081(8) 0.0080(9)
C13D 0.0311(12) 0.0267(11) 0.0235(11) 0.0061(9) 0.0017(9) 0.0099(10)
C14D 0.0265(12) 0.0242(11) 0.0394(13) 0.0112(10) -0.0061(10) 0.0006(9)
C15D 0.0245(11) 0.0303(12) 0.0467(14) 0.0222(11) 0.0071(10) 0.0023(9)
C16D 0.0238(11) 0.0245(11) 0.0292(11) 0.0157(9) 0.0066(8) 0.0070(9)
C21D 0.0230(10) 0.0185(10) 0.0211(10) 0.0089(8) 0.0046(8) -0.0009(8)
C22D 0.0312(12) 0.0362(12) 0.0271(11) 0.0128(10) 0.0096(9) 0.0076(10)
C23D 0.0503(16) 0.0470(15) 0.0304(13) 0.0134(11) 0.0228(11) 0.0081(12)
C24D 0.0684(18) 0.0454(15) 0.0208(11) 0.0154(11) 0.0101(12) -0.0034(13)
C25D 0.0498(15) 0.0352(13) 0.0262(12) 0.0170(10) -0.0040(11) -0.0010(11)
C26D 0.0287(11) 0.0243(11) 0.0257(11) 0.0118(9) 0.0022(9) 0.0010(9)
C31D 0.0184(10) 0.0204(10) 0.0170(9) 0.0055(8) 0.0010(7) 0.0030(8)
C32D 0.0276(11) 0.0269(11) 0.0283(11) 0.0107(9) 0.0033(9) 0.0069(9)
C33D 0.0357(13) 0.0261(12) 0.0337(12) 0.0025(10) -0.0026(10) 0.0128(10)
C34D 0.0219(12) 0.0464(15) 0.0312(12) -0.0014(11) 0.0033(9) 0.0148(11)
C35D 0.0217(11) 0.0412(14) 0.0340(12) 0.0087(10) 0.0102(9) 0.0038(10)
C36D 0.0249(11) 0.0264(11) 0.0247(10) 0.0094(9) 0.0079(8) 0.0052(9)
C41D 0.0201(10) 0.0237(10) 0.0204(10) 0.0104(8) 0.0103(8) 0.0076(8)
C42D 0.0282(11) 0.0256(11) 0.0252(11) 0.0108(9) 0.0080(9) 0.0084(9)
C43D 0.0362(13) 0.0219(11) 0.0330(12) 0.0084(9) 0.0126(10) 0.0033(10)
C44D 0.0457(15) 0.0259(12) 0.0471(14) 0.0215(11) 0.0187(12) 0.0129(11)
C45D 0.0372(13) 0.0402(14) 0.0448(14) 0.0300(12) 0.0094(11) 0.0143(11)
C46D 0.0253(11) 0.0300(11) 0.0286(11) 0.0157(9) 0.0067(9) 0.0059(9)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 C2 2.0518(19) . ?
Rh1 N3' 2.0902(15) . ?
Rh1 C2B 2.136(2) . ?
Rh1 C1B 2.1671(19) . ?
Rh1 C6B 2.175(2) . ?
Rh1 C5B 2.2040(19) . ?
N1 C2 1.360(2) . ?
N1 C5 1.386(2) . ?
N1 C6 1.444(2) . ?
C2 N3 1.356(2) . ?
N3 C4 1.387(3) . ?
N3 C1A 1.461(2) . ?
C4 C5 1.338(3) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C1A C4' 1.490(3) . ?
C1A H1A1 0.9900 . ?
C1A H1A2 0.9900 . ?
N1' N2' 1.330(2) . ?
N1' C5' 1.347(3) . ?
N1' C6' 1.474(3) . ?
N2' N3' 1.323(2) . ?
N3' C4' 1.352(2) . ?
C4' C5' 1.362(3) . ?
C5' H5' 0.9500 . ?
C6 C11 1.392(3) . ?
C6 C7 1.395(3) . ?
C7 C8 1.390(3) . ?
C7 C12 1.499(3) . ?
C8 C9 1.377(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.389(3) . ?
C9 C13 1.514(3) . ?
C10 C11 1.392(3) . ?
C10 H10 0.9500 . ?
C11 C14 1.503(3) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13G 0.9800 . ?
C13 H13E 0.9800 . ?
C13 H13F 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C6' C7' 1.500(3) . ?
C6' H6'1 0.9900 . ?
C6' H6'2 0.9900 . ?
C7' C8' 1.388(3) . ?
C7' C12' 1.392(3) . ?
C8' C9' 1.376(3) . ?
C8' H8' 0.9500 . ?
C9' C10' 1.391(3) . ?
C9' H9' 0.9500 . ?
C10' O1' 1.366(3) . ?
C10' C11' 1.384(3) . ?
C11' C12' 1.385(3) . ?
C11' H11' 0.9500 . ?
C12' H12' 0.9500 . ?
C13' O1' 1.420(3) . ?
C13' H13A 0.9800 . ?
C13' H13B 0.9800 . ?
C13' H13C 0.9800 . ?
C5B C6B 1.374(3) . ?
C5B C4B 1.516(3) . ?
C5B H5B 0.9500 . ?
C6B C7B 1.504(3) . ?
C6B H6B 0.9500 . ?
C7B C8B 1.526(4) . ?
C7B H71B 0.9900 . ?
C7B H72B 0.9900 . ?
C8B C1B 1.517(3) . ?
C8B H82B 0.9900 . ?
C8B H81B 0.9900 . ?
C1B C2B 1.390(3) . ?
C1B H1B 0.9500 . ?
C2B C3B 1.507(3) . ?
C2B H2B 0.9500 . ?
C3B C4B 1.537(3) . ?
C3B H31B 0.9900 . ?
C3B H32B 0.9900 . ?
C4B H41B 0.9900 . ?
C4B H42B 0.9900 . ?
B1D C21D 1.643(3) . ?
B1D C11D 1.646(3) . ?
B1D C31D 1.647(3) . ?
B1D C41D 1.653(3) . ?
C11D C16D 1.402(3) . ?
C11D C12D 1.403(3) . ?
C12D C13D 1.385(3) . ?
C12D H12D 0.9500 . ?
C13D C14D 1.379(3) . ?
C13D H13D 0.9500 . ?
C14D C15D 1.376(3) . ?
C14D H14D 0.9500 . ?
C15D C16D 1.398(3) . ?
C15D H15D 0.9500 . ?
C16D H16D 0.9500 . ?
C21D C26D 1.399(3) . ?
C21D C22D 1.404(3) . ?
C22D C23D 1.384(3) . ?
C22D H22D 0.9500 . ?
C23D C24D 1.378(4) . ?
C23D H23D 0.9500 . ?
C24D C25D 1.380(4) . ?
C24D H24D 0.9500 . ?
C25D C26D 1.388(3) . ?
C25D H25D 0.9500 . ?
C26D H26D 0.9500 . ?
C31D C36D 1.396(3) . ?
C31D C32D 1.405(3) . ?
C32D C33D 1.383(3) . ?
C32D H32D 0.9500 . ?
C33D C34D 1.385(4) . ?
C33D H33D 0.9500 . ?
C34D C35D 1.371(3) . ?
C34D H34D 0.9500 . ?
C35D C36D 1.388(3) . ?
C35D H35D 0.9500 . ?
C36D H36D 0.9500 . ?
C41D C46D 1.396(3) . ?
C41D C42D 1.406(3) . ?
C42D C43D 1.386(3) . ?
C42D H42D 0.9500 . ?
C43D C44D 1.382(3) . ?
C43D H43D 0.9500 . ?
C44D C45D 1.378(3) . ?
C44D H44D 0.9500 . ?
C45D C46D 1.390(3) . ?
C45D H45D 0.9500 . ?
C46D H46D 0.9500 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Rh1 N3' 85.12(7) . . ?
C2 Rh1 C2B 95.06(8) . . ?
N3' Rh1 C2B 149.72(8) . . ?
C2 Rh1 C1B 98.84(8) . . ?
N3' Rh1 C1B 171.65(8) . . ?
C2B Rh1 C1B 37.69(9) . . ?
C2 Rh1 C6B 158.57(8) . . ?
N3' Rh1 C6B 92.44(7) . . ?
C2B Rh1 C6B 97.62(9) . . ?
C1B Rh1 C6B 81.18(8) . . ?
C2 Rh1 C5B 163.98(8) . . ?
N3' Rh1 C5B 89.56(7) . . ?
C2B Rh1 C5B 82.00(8) . . ?
C1B Rh1 C5B 88.48(8) . . ?
C6B Rh1 C5B 36.57(8) . . ?
C2 N1 C5 111.61(15) . . ?
C2 N1 C6 126.85(16) . . ?
C5 N1 C6 121.51(16) . . ?
N3 C2 N1 103.25(16) . . ?
N3 C2 Rh1 122.54(14) . . ?
N1 C2 Rh1 133.28(13) . . ?
C2 N3 C4 112.01(16) . . ?
C2 N3 C1A 123.10(16) . . ?
C4 N3 C1A 124.81(16) . . ?
C5 C4 N3 106.34(17) . . ?
C5 C4 H4 126.8 . . ?
N3 C4 H4 126.8 . . ?
C4 C5 N1 106.80(17) . . ?
C4 C5 H5 126.6 . . ?
N1 C5 H5 126.6 . . ?
N3 C1A C4' 110.93(16) . . ?
N3 C1A H1A1 109.5 . . ?
C4' C1A H1A1 109.5 . . ?
N3 C1A H1A2 109.5 . . ?
C4' C1A H1A2 109.5 . . ?
H1A1 C1A H1A2 108.0 . . ?
N2' N1' C5' 111.91(16) . . ?
N2' N1' C6' 119.44(16) . . ?
C5' N1' C6' 128.34(17) . . ?
N3' N2' N1' 105.72(15) . . ?
N2' N3' C4' 109.98(15) . . ?
N2' N3' Rh1 126.28(12) . . ?
C4' N3' Rh1 123.55(13) . . ?
N3' C4' C5' 107.66(17) . . ?
N3' C4' C1A 120.63(17) . . ?
C5' C4' C1A 131.68(18) . . ?
N1' C5' C4' 104.73(17) . . ?
N1' C5' H5' 127.6 . . ?
C4' C5' H5' 127.6 . . ?
C11 C6 C7 122.89(18) . . ?
C11 C6 N1 119.34(17) . . ?
C7 C6 N1 117.73(17) . . ?
C8 C7 C6 117.1(2) . . ?
C8 C7 C12 120.42(19) . . ?
C6 C7 C12 122.43(18) . . ?
C9 C8 C7 122.1(2) . . ?
C9 C8 H8 118.9 . . ?
C7 C8 H8 118.9 . . ?
C8 C9 C10 118.79(19) . . ?
C8 C9 C13 120.3(2) . . ?
C10 C9 C13 120.8(2) . . ?
C9 C10 C11 121.8(2) . . ?
C9 C10 H10 119.1 . . ?
C11 C10 H10 119.1 . . ?
C10 C11 C6 117.2(2) . . ?
C10 C11 C14 121.2(2) . . ?
C6 C11 C14 121.62(18) . . ?
C7 C12 H12A 109.5 . . ?
C7 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C7 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C9 C13 H13G 109.5 . . ?
C9 C13 H13E 109.5 . . ?
H13G C13 H13E 109.5 . . ?
C9 C13 H13F 109.5 . . ?
H13G C13 H13F 109.5 . . ?
H13E C13 H13F 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N1' C6' C7' 110.94(17) . . ?
N1' C6' H6'1 109.5 . . ?
C7' C6' H6'1 109.5 . . ?
N1' C6' H6'2 109.5 . . ?
C7' C6' H6'2 109.5 . . ?
H6'1 C6' H6'2 108.0 . . ?
C8' C7' C12' 118.1(2) . . ?
C8' C7' C6' 121.28(19) . . ?
C12' C7' C6' 120.58(19) . . ?
C9' C8' C7' 121.2(2) . . ?
C9' C8' H8' 119.4 . . ?
C7' C8' H8' 119.4 . . ?
C8' C9' C10' 120.0(2) . . ?
C8' C9' H9' 120.0 . . ?
C10' C9' H9' 120.0 . . ?
O1' C10' C11' 124.5(2) . . ?
O1' C10' C9' 115.67(19) . . ?
C11' C10' C9' 119.8(2) . . ?
C10' C11' C12' 119.5(2) . . ?
C10' C11' H11' 120.3 . . ?
C12' C11' H11' 120.3 . . ?
C11' C12' C7' 121.40(19) . . ?
C11' C12' H12' 119.3 . . ?
C7' C12' H12' 119.3 . . ?
O1' C13' H13A 109.5 . . ?
O1' C13' H13B 109.5 . . ?
H13A C13' H13B 109.5 . . ?
O1' C13' H13C 109.5 . . ?
H13A C13' H13C 109.5 . . ?
H13B C13' H13C 109.5 . . ?
C10' O1' C13' 117.13(18) . . ?
C6B C5B C4B 126.04(19) . . ?
C6B C5B Rh1 70.56(11) . . ?
C4B C5B Rh1 111.08(14) . . ?
C6B C5B H5B 117.0 . . ?
C4B C5B H5B 117.0 . . ?
Rh1 C5B H5B 88.3 . . ?
C5B C6B C7B 126.0(2) . . ?
C5B C6B Rh1 72.87(12) . . ?
C7B C6B Rh1 108.74(15) . . ?
C5B C6B H6B 117.0 . . ?
C7B C6B H6B 117.0 . . ?
Rh1 C6B H6B 88.3 . . ?
C6B C7B C8B 112.45(19) . . ?
C6B C7B H71B 109.1 . . ?
C8B C7B H71B 109.1 . . ?
C6B C7B H72B 109.1 . . ?
C8B C7B H72B 109.1 . . ?
H71B C7B H72B 107.8 . . ?
C1B C8B C7B 112.88(18) . . ?
C1B C8B H82B 109.0 . . ?
C7B C8B H82B 109.0 . . ?
C1B C8B H81B 109.0 . . ?
C7B C8B H81B 109.0 . . ?
H82B C8B H81B 107.8 . . ?
C2B C1B C8B 124.1(2) . . ?
C2B C1B Rh1 69.93(11) . . ?
C8B C1B Rh1 112.00(15) . . ?
C2B C1B H1B 117.9 . . ?
C8B C1B H1B 117.9 . . ?
Rh1 C1B H1B 88.1 . . ?
C1B C2B C3B 124.7(2) . . ?
C1B C2B Rh1 72.38(12) . . ?
C3B C2B Rh1 108.90(14) . . ?
C1B C2B H2B 117.6 . . ?
C3B C2B H2B 117.6 . . ?
Rh1 C2B H2B 88.7 . . ?
C2B C3B C4B 114.50(19) . . ?
C2B C3B H31B 108.6 . . ?
C4B C3B H31B 108.6 . . ?
C2B C3B H32B 108.6 . . ?
C4B C3B H32B 108.6 . . ?
H31B C3B H32B 107.6 . . ?
C5B C4B C3B 112.74(17) . . ?
C5B C4B H41B 109.0 . . ?
C3B C4B H41B 109.0 . . ?
C5B C4B H42B 109.0 . . ?
C3B C4B H42B 109.0 . . ?
H41B C4B H42B 107.8 . . ?
C21D B1D C11D 111.91(16) . . ?
C21D B1D C31D 111.62(16) . . ?
C11D B1D C31D 106.21(15) . . ?
C21D B1D C41D 107.37(15) . . ?
C11D B1D C41D 110.78(15) . . ?
C31D B1D C41D 108.96(15) . . ?
C16D C11D C12D 115.01(18) . . ?
C16D C11D B1D 125.87(17) . . ?
C12D C11D B1D 119.11(17) . . ?
C13D C12D C11D 123.57(19) . . ?
C13D C12D H12D 118.2 . . ?
C11D C12D H12D 118.2 . . ?
C14D C13D C12D 119.5(2) . . ?
C14D C13D H13D 120.2 . . ?
C12D C13D H13D 120.2 . . ?
C15D C14D C13D 119.3(2) . . ?
C15D C14D H14D 120.3 . . ?
C13D C14D H14D 120.3 . . ?
C14D C15D C16D 120.7(2) . . ?
C14D C15D H15D 119.7 . . ?
C16D C15D H15D 119.7 . . ?
C15D C16D C11D 121.9(2) . . ?
C15D C16D H16D 119.1 . . ?
C11D C16D H16D 119.1 . . ?
C26D C21D C22D 114.62(18) . . ?
C26D C21D B1D 124.86(18) . . ?
C22D C21D B1D 120.46(17) . . ?
C23D C22D C21D 123.1(2) . . ?
C23D C22D H22D 118.5 . . ?
C21D C22D H22D 118.5 . . ?
C24D C23D C22D 120.2(2) . . ?
C24D C23D H23D 119.9 . . ?
C22D C23D H23D 119.9 . . ?
C23D C24D C25D 119.0(2) . . ?
C23D C24D H24D 120.5 . . ?
C25D C24D H24D 120.5 . . ?
C24D C25D C26D 120.1(2) . . ?
C24D C25D H25D 119.9 . . ?
C26D C25D H25D 119.9 . . ?
C25D C26D C21D 123.0(2) . . ?
C25D C26D H26D 118.5 . . ?
C21D C26D H26D 118.5 . . ?
C36D C31D C32D 115.12(18) . . ?
C36D C31D B1D 124.03(17) . . ?
C32D C31D B1D 120.82(17) . . ?
C33D C32D C31D 122.7(2) . . ?
C33D C32D H32D 118.6 . . ?
C31D C32D H32D 118.6 . . ?
C32D C33D C34D 120.1(2) . . ?
C32D C33D H33D 120.0 . . ?
C34D C33D H33D 120.0 . . ?
C35D C34D C33D 118.8(2) . . ?
C35D C34D H34D 120.6 . . ?
C33D C34D H34D 120.6 . . ?
C34D C35D C36D 120.7(2) . . ?
C34D C35D H35D 119.7 . . ?
C36D C35D H35D 119.7 . . ?
C35D C36D C31D 122.5(2) . . ?
C35D C36D H36D 118.8 . . ?
C31D C36D H36D 118.8 . . ?
C46D C41D C42D 114.89(18) . . ?
C46D C41D B1D 125.72(18) . . ?
C42D C41D B1D 119.35(17) . . ?
C43D C42D C41D 122.7(2) . . ?
C43D C42D H42D 118.6 . . ?
C41D C42D H42D 118.6 . . ?
C44D C43D C42D 120.2(2) . . ?
C44D C43D H43D 119.9 . . ?
C42D C43D H43D 119.9 . . ?
C45D C44D C43D 119.1(2) . . ?
C45D C44D H44D 120.5 . . ?
C43D C44D H44D 120.5 . . ?
C44D C45D C46D 120.0(2) . . ?
C44D C45D H45D 120.0 . . ?
C46D C45D H45D 120.0 . . ?
C45D C46D C41D 123.1(2) . . ?
C45D C46D H46D 118.4 . . ?
C41D C46D H46D 118.4 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 C2 N3 -0.1(2) . . . . ?
C6 N1 C2 N3 178.20(17) . . . . ?
C5 N1 C2 Rh1 168.69(15) . . . . ?
C6 N1 C2 Rh1 -13.0(3) . . . . ?
N3' Rh1 C2 N3 32.39(15) . . . . ?
C2B Rh1 C2 N3 -117.21(16) . . . . ?
C1B Rh1 C2 N3 -155.01(16) . . . . ?
C6B Rh1 C2 N3 116.6(2) . . . . ?
C5B Rh1 C2 N3 -38.6(4) . . . . ?
N3' Rh1 C2 N1 -134.60(19) . . . . ?
C2B Rh1 C2 N1 75.79(19) . . . . ?
C1B Rh1 C2 N1 38.0(2) . . . . ?
C6B Rh1 C2 N1 -50.4(3) . . . . ?
C5B Rh1 C2 N1 154.4(2) . . . . ?
N1 C2 N3 C4 0.0(2) . . . . ?
Rh1 C2 N3 C4 -170.33(13) . . . . ?
N1 C2 N3 C1A 176.75(17) . . . . ?
Rh1 C2 N3 C1A 6.4(3) . . . . ?
C2 N3 C4 C5 0.1(2) . . . . ?
C1A N3 C4 C5 -176.60(18) . . . . ?
N3 C4 C5 N1 -0.1(2) . . . . ?
C2 N1 C5 C4 0.1(2) . . . . ?
C6 N1 C5 C4 -178.24(17) . . . . ?
C2 N3 C1A C4' -54.9(2) . . . . ?
C4 N3 C1A C4' 121.5(2) . . . . ?
C5' N1' N2' N3' -0.2(2) . . . . ?
C6' N1' N2' N3' -174.42(16) . . . . ?
N1' N2' N3' C4' 0.0(2) . . . . ?
N1' N2' N3' Rh1 175.12(12) . . . . ?
C2 Rh1 N3' N2' 148.09(16) . . . . ?
C2B Rh1 N3' N2' -120.23(18) . . . . ?
C1B Rh1 N3' N2' 29.4(6) . . . . ?
C6B Rh1 N3' N2' -10.57(16) . . . . ?
C5B Rh1 N3' N2' -47.04(16) . . . . ?
C2 Rh1 N3' C4' -37.45(16) . . . . ?
C2B Rh1 N3' C4' 54.2(2) . . . . ?
C1B Rh1 N3' C4' -156.2(4) . . . . ?
C6B Rh1 N3' C4' 163.89(16) . . . . ?
C5B Rh1 N3' C4' 127.42(16) . . . . ?
N2' N3' C4' C5' 0.2(2) . . . . ?
Rh1 N3' C4' C5' -175.07(13) . . . . ?
N2' N3' C4' C1A 178.69(17) . . . . ?
Rh1 N3' C4' C1A 3.4(3) . . . . ?
N3 C1A C4' N3' 48.3(3) . . . . ?
N3 C1A C4' C5' -133.6(2) . . . . ?
N2' N1' C5' C4' 0.3(2) . . . . ?
C6' N1' C5' C4' 173.88(19) . . . . ?
N3' C4' C5' N1' -0.3(2) . . . . ?
C1A C4' C5' N1' -178.6(2) . . . . ?
C2 N1 C6 C11 77.2(3) . . . . ?
C5 N1 C6 C11 -104.6(2) . . . . ?
C2 N1 C6 C7 -105.1(2) . . . . ?
C5 N1 C6 C7 73.0(2) . . . . ?
C11 C6 C7 C8 2.3(3) . . . . ?
N1 C6 C7 C8 -175.31(17) . . . . ?
C11 C6 C7 C12 -178.8(2) . . . . ?
N1 C6 C7 C12 3.7(3) . . . . ?
C6 C7 C8 C9 -0.3(3) . . . . ?
C12 C7 C8 C9 -179.3(2) . . . . ?
C7 C8 C9 C10 -2.2(3) . . . . ?
C7 C8 C9 C13 174.6(2) . . . . ?
C8 C9 C10 C11 2.9(3) . . . . ?
C13 C9 C10 C11 -173.8(2) . . . . ?
C9 C10 C11 C6 -1.1(3) . . . . ?
C9 C10 C11 C14 178.5(2) . . . . ?
C7 C6 C11 C10 -1.6(3) . . . . ?
N1 C6 C11 C10 175.97(18) . . . . ?
C7 C6 C11 C14 178.9(2) . . . . ?
N1 C6 C11 C14 -3.6(3) . . . . ?
N2' N1' C6' C7' 87.4(2) . . . . ?
C5' N1' C6' C7' -85.7(3) . . . . ?
N1' C6' C7' C8' -94.8(2) . . . . ?
N1' C6' C7' C12' 82.7(2) . . . . ?
C12' C7' C8' C9' -1.0(3) . . . . ?
C6' C7' C8' C9' 176.6(2) . . . . ?
C7' C8' C9' C10' -0.1(3) . . . . ?
C8' C9' C10' O1' -179.9(2) . . . . ?
C8' C9' C10' C11' 1.1(3) . . . . ?
O1' C10' C11' C12' -179.91(19) . . . . ?
C9' C10' C11' C12' -0.9(3) . . . . ?
C10' C11' C12' C7' -0.2(3) . . . . ?
C8' C7' C12' C11' 1.1(3) . . . . ?
C6' C7' C12' C11' -176.47(19) . . . . ?
C11' C10' O1' C13' -8.9(3) . . . . ?
C9' C10' O1' C13' 172.1(2) . . . . ?
C2 Rh1 C5B C6B 165.1(2) . . . . ?
N3' Rh1 C5B C6B 94.70(13) . . . . ?
C2B Rh1 C5B C6B -114.47(14) . . . . ?
C1B Rh1 C5B C6B -77.19(14) . . . . ?
C2 Rh1 C5B C4B -72.7(3) . . . . ?
N3' Rh1 C5B C4B -143.12(15) . . . . ?
C2B Rh1 C5B C4B 7.72(15) . . . . ?
C1B Rh1 C5B C4B 45.00(15) . . . . ?
C6B Rh1 C5B C4B 122.2(2) . . . . ?
C4B C5B C6B C7B -1.4(3) . . . . ?
Rh1 C5B C6B C7B 101.0(2) . . . . ?
C4B C5B C6B Rh1 -102.4(2) . . . . ?
C2 Rh1 C6B C5B -168.81(18) . . . . ?
N3' Rh1 C6B C5B -85.96(13) . . . . ?
C2B Rh1 C6B C5B 65.42(14) . . . . ?
C1B Rh1 C6B C5B 99.45(14) . . . . ?
C2 Rh1 C6B C7B 68.2(3) . . . . ?
N3' Rh1 C6B C7B 151.04(16) . . . . ?
C2B Rh1 C6B C7B -57.58(17) . . . . ?
C1B Rh1 C6B C7B -23.55(17) . . . . ?
C5B Rh1 C6B C7B -123.0(2) . . . . ?
C5B C6B C7B C8B -43.3(3) . . . . ?
Rh1 C6B C7B C8B 38.8(2) . . . . ?
C6B C7B C8B C1B -36.0(3) . . . . ?
C7B C8B C1B C2B 94.8(3) . . . . ?
C7B C8B C1B Rh1 14.8(2) . . . . ?
C2 Rh1 C1B C2B 86.83(13) . . . . ?
N3' Rh1 C1B C2B -155.3(4) . . . . ?
C6B Rh1 C1B C2B -114.86(14) . . . . ?
C5B Rh1 C1B C2B -78.85(13) . . . . ?
C2 Rh1 C1B C8B -153.41(16) . . . . ?
N3' Rh1 C1B C8B -35.6(6) . . . . ?
C2B Rh1 C1B C8B 119.8(2) . . . . ?
C6B Rh1 C1B C8B 4.90(16) . . . . ?
C5B Rh1 C1B C8B 40.91(16) . . . . ?
C8B C1B C2B C3B -2.4(3) . . . . ?
Rh1 C1B C2B C3B 101.2(2) . . . . ?
C8B C1B C2B Rh1 -103.6(2) . . . . ?
C2 Rh1 C2B C1B -97.92(13) . . . . ?
N3' Rh1 C2B C1B 173.10(13) . . . . ?
C6B Rh1 C2B C1B 64.77(14) . . . . ?
C5B Rh1 C2B C1B 97.94(13) . . . . ?
C2 Rh1 C2B C3B 140.55(16) . . . . ?
N3' Rh1 C2B C3B 51.6(2) . . . . ?
C1B Rh1 C2B C3B -121.5(2) . . . . ?
C6B Rh1 C2B C3B -56.77(17) . . . . ?
C5B Rh1 C2B C3B -23.59(16) . . . . ?
C1B C2B C3B C4B -44.5(3) . . . . ?
Rh1 C2B C3B C4B 36.8(2) . . . . ?
C6B C5B C4B C3B 90.5(3) . . . . ?
Rh1 C5B C4B C3B 9.8(2) . . . . ?
C2B C3B C4B C5B -31.2(3) . . . . ?
C21D B1D C11D C16D -4.0(3) . . . . ?
C31D B1D C11D C16D -125.99(19) . . . . ?
C41D B1D C11D C16D 115.8(2) . . . . ?
C21D B1D C11D C12D 175.30(16) . . . . ?
C31D B1D C11D C12D 53.3(2) . . . . ?
C41D B1D C11D C12D -64.9(2) . . . . ?
C16D C11D C12D C13D -1.0(3) . . . . ?
B1D C11D C12D C13D 179.66(18) . . . . ?
C11D C12D C13D C14D 0.5(3) . . . . ?
C12D C13D C14D C15D 0.2(3) . . . . ?
C13D C14D C15D C16D -0.2(3) . . . . ?
C14D C15D C16D C11D -0.4(3) . . . . ?
C12D C11D C16D C15D 1.0(3) . . . . ?
B1D C11D C16D C15D -179.76(18) . . . . ?
C11D B1D C21D C26D -117.9(2) . . . . ?
C31D B1D C21D C26D 1.0(3) . . . . ?
C41D B1D C21D C26D 120.3(2) . . . . ?
C11D B1D C21D C22D 65.1(2) . . . . ?
C31D B1D C21D C22D -176.02(18) . . . . ?
C41D B1D C21D C22D -56.7(2) . . . . ?
C26D C21D C22D C23D 1.1(3) . . . . ?
B1D C21D C22D C23D 178.4(2) . . . . ?
C21D C22D C23D C24D -0.9(4) . . . . ?
C22D C23D C24D C25D -0.2(4) . . . . ?
C23D C24D C25D C26D 1.2(4) . . . . ?
C24D C25D C26D C21D -1.0(3) . . . . ?
C22D C21D C26D C25D -0.2(3) . . . . ?
B1D C21D C26D C25D -177.29(19) . . . . ?
C21D B1D C31D C36D 120.7(2) . . . . ?
C11D B1D C31D C36D -117.1(2) . . . . ?
C41D B1D C31D C36D 2.3(3) . . . . ?
C21D B1D C31D C32D -61.5(2) . . . . ?
C11D B1D C31D C32D 60.7(2) . . . . ?
C41D B1D C31D C32D -179.91(17) . . . . ?
C36D C31D C32D C33D -1.7(3) . . . . ?
B1D C31D C32D C33D -179.67(19) . . . . ?
C31D C32D C33D C34D 2.6(3) . . . . ?
C32D C33D C34D C35D -0.9(3) . . . . ?
C33D C34D C35D C36D -1.4(3) . . . . ?
C34D C35D C36D C31D 2.2(3) . . . . ?
C32D C31D C36D C35D -0.7(3) . . . . ?
B1D C31D C36D C35D 177.23(19) . . . . ?
C21D B1D C41D C46D 135.57(19) . . . . ?
C11D B1D C41D C46D 13.1(3) . . . . ?
C31D B1D C41D C46D -103.4(2) . . . . ?
C21D B1D C41D C42D -46.9(2) . . . . ?
C11D B1D C41D C42D -169.32(16) . . . . ?
C31D B1D C41D C42D 74.2(2) . . . . ?
C46D C41D C42D C43D -0.5(3) . . . . ?
B1D C41D C42D C43D -178.36(18) . . . . ?
C41D C42D C43D C44D -0.5(3) . . . . ?
C42D C43D C44D C45D 1.0(3) . . . . ?
C43D C44D C45D C46D -0.4(3) . . . . ?
C44D C45D C46D C41D -0.7(3) . . . . ?
C42D C41D C46D C45D 1.1(3) . . . . ?
B1D C41D C46D C45D 178.80(19) . . . . ?
_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max 0.379
_refine_diff_density_min -0.393
_refine_diff_density_rms 0.051
_database_code_depnum_ccdc_archive 'CCDC 934038'
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_khuong7_fulldata
#TrackingRef 'Khuong7_Deposition_221May12.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C25 H25 N5 O3 Rh, C24 H20 B'
_chemical_formula_sum 'C49 H45 B N5 O3 Rh'
_chemical_formula_weight 865.62
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M P2(1)/c
_symmetry_space_group_name_Hall '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 17.012(4)
_cell_length_b 16.520(4)
_cell_length_c 14.645(2)
_cell_angle_alpha 90.00
_cell_angle_beta 90.01(1)
_cell_angle_gamma 90.00
_cell_volume 4115.8(15)
_cell_formula_units_Z 4
_cell_measurement_temperature 150(2)
_cell_measurement_reflns_used 4501
_cell_measurement_theta_min 2.437
_cell_measurement_theta_max 23.121
_exptl_crystal_description 'Square plates'
_exptl_crystal_colour 'Dark red'
_exptl_crystal_size_max 0.29
_exptl_crystal_size_mid 0.23
_exptl_crystal_size_min 0.09
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.397
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1792
_exptl_absorpt_coefficient_mu 0.465
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.8754
_exptl_absorpt_correction_T_max 0.9598
_exptl_absorpt_process_details 'SADABS (Bruker, 2001)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 150(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker kappa APEXII CCD Diffractometer'
_diffrn_measurement_method '\f scans, and \w scans with \k offsets'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 29045
_diffrn_reflns_av_R_equivalents 0.0724
_diffrn_reflns_av_sigmaI/netI 0.0666
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_h_max 20
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_theta_min 3.03
_diffrn_reflns_theta_max 25.00
_reflns_number_total 7168
_reflns_number_gt 5248
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2007)'
_computing_cell_refinement 'APEX2 (Bruker, 2007)'
_computing_data_reduction 'APEX2 (Bruker, 2007)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
he unit cell angles ndicate the crystal system to be orthorhobmic,but the structure solution and refinement could be done only in the Monoclinic space group P2(1)/c.
The ligand exhibited orientational disorder for the part containing phenyl
ring with the O-methoxy substitution. The two positions were found to have
occupancies of ~ 80% (C7'/c8'/c9'/c10'/c11'/c12'/o1'/c13') and ~20% (for
the double primed labelled atoms of this group). The atoms in the minor site
were kept isotropic in the least-squares refinement.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0283P)^2^+3.1794P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 7168
_refine_ls_number_parameters 549
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0654
_refine_ls_R_factor_gt 0.0377
_refine_ls_wR_factor_ref 0.0906
_refine_ls_wR_factor_gt 0.0791
_refine_ls_goodness_of_fit_ref 0.998
_refine_ls_restrained_S_all 0.998
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 1.011510(15) 0.545799(15) 0.901674(17) 0.02417(9) Uani 1 1 d . . .
N1 N 1.12232(15) 0.69338(16) 0.91922(17) 0.0256(6) Uani 1 1 d . . .
C2 C 1.05098(19) 0.65672(19) 0.9345(2) 0.0241(7) Uani 1 1 d . . .
N3 N 1.00494(15) 0.71245(16) 0.97591(17) 0.0258(6) Uani 1 1 d . . .
C4 C 1.0472(2) 0.7812(2) 0.9860(2) 0.0318(8) Uani 1 1 d . . .
H4 H 1.0290 0.8297 1.0137 0.038 Uiso 1 1 calc R . .
C5 C 1.1201(2) 0.7694(2) 0.9499(2) 0.0319(8) Uani 1 1 d . . .
H5 H 1.1615 0.8079 0.9470 0.038 Uiso 1 1 calc R . .
C1A C 0.92388(19) 0.7018(2) 1.0114(2) 0.0297(8) Uani 1 1 d . . .
H1A H 0.9265 0.6726 1.0703 0.036 Uiso 1 1 calc R . .
H1B H 0.9010 0.7559 1.0234 0.036 Uiso 1 1 calc R . .
N1' N 0.77388(16) 0.60689(17) 0.87567(17) 0.0278(6) Uani 1 1 d . B .
N2' N 0.83606(16) 0.55981(16) 0.86085(17) 0.0272(6) Uani 1 1 d . . .
N3' N 0.89634(16) 0.59133(16) 0.90655(17) 0.0252(6) Uani 1 1 d . . .
C4' C 0.87141(19) 0.6573(2) 0.9493(2) 0.0267(8) Uani 1 1 d . . .
C5' C 0.79288(19) 0.6680(2) 0.9291(2) 0.0278(8) Uani 1 1 d . . .
H5' H 0.7595 0.7104 0.9495 0.033 Uiso 1 1 calc R . .
C6 C 1.19272(19) 0.66173(19) 0.8751(2) 0.0253(7) Uani 1 1 d . . .
C7 C 1.2576(2) 0.6403(2) 0.9284(2) 0.0303(8) Uani 1 1 d . . .
C8 C 1.3271(2) 0.6166(2) 0.8840(2) 0.0355(9) Uani 1 1 d . . .
H8 H 1.3715 0.6022 0.9199 0.043 Uiso 1 1 calc R . .
C9 C 1.3333(2) 0.6135(2) 0.7901(3) 0.0392(9) Uani 1 1 d . . .
C10 C 1.2662(2) 0.6343(2) 0.7400(2) 0.0404(9) Uani 1 1 d . . .
H10 H 1.2686 0.6310 0.6753 0.048 Uiso 1 1 calc R . .
C11 C 1.1952(2) 0.6599(2) 0.7809(2) 0.0317(8) Uani 1 1 d . . .
C12 C 1.2525(2) 0.6423(3) 1.0311(2) 0.0453(10) Uani 1 1 d . . .
H12A H 1.2380 0.6968 1.0512 0.068 Uiso 1 1 calc R . .
H12B H 1.3036 0.6276 1.0572 0.068 Uiso 1 1 calc R . .
H12C H 1.2126 0.6036 1.0517 0.068 Uiso 1 1 calc R . .
C13 C 1.4110(2) 0.5886(3) 0.7445(3) 0.0590(12) Uani 1 1 d . . .
H13A H 1.4552 0.6088 0.7809 0.089 Uiso 1 1 calc R . .
H13B H 1.4135 0.6118 0.6830 0.089 Uiso 1 1 calc R . .
H13C H 1.4138 0.5295 0.7406 0.089 Uiso 1 1 calc R . .
C14 C 1.1257(2) 0.6890(3) 0.7251(2) 0.0490(11) Uani 1 1 d . . .
H14A H 1.0800 0.6547 0.7377 0.073 Uiso 1 1 calc R . .
H14B H 1.1386 0.6861 0.6600 0.073 Uiso 1 1 calc R . .
H14C H 1.1135 0.7452 0.7415 0.073 Uiso 1 1 calc R . .
C6' C 0.69534(19) 0.5913(2) 0.8328(2) 0.0344(9) Uani 1 1 d . . .
H6'1 H 0.6923 0.5339 0.8133 0.041 Uiso 1 1 calc R A 1
H6'2 H 0.6894 0.6256 0.7778 0.041 Uiso 1 1 calc R A 1
C7' C 0.6274(2) 0.6097(3) 0.9008(3) 0.030(6) Uani 0.703(6) 1 d PG B 1
C8' C 0.5906(3) 0.6848(2) 0.9043(3) 0.0369(16) Uani 0.703(6) 1 d PG B 1
H8' H 0.6020 0.7246 0.8594 0.044 Uiso 0.703(6) 1 calc PR B 1
C9' C 0.5372(2) 0.70167(18) 0.9736(3) 0.0401(16) Uani 0.703(6) 1 d PG B 1
H9' H 0.5121 0.7530 0.9760 0.048 Uiso 0.703(6) 1 calc PR B 1
C10' C 0.52060(17) 0.6435(2) 1.0393(2) 0.0325(14) Uani 0.703(6) 1 d PG B 1
C11' C 0.5574(2) 0.5684(2) 1.0358(2) 0.0484(18) Uani 0.703(6) 1 d PG B 1
H11' H 0.5460 0.5286 1.0808 0.058 Uiso 0.703(6) 1 calc PR B 1
C12' C 0.6108(2) 0.5515(2) 0.9666(3) 0.0488(16) Uani 0.703(6) 1 d PG B 1
H12' H 0.6359 0.5002 0.9642 0.059 Uiso 0.703(6) 1 calc PR B 1
O1' O 0.4701(2) 0.6529(3) 1.1141(3) 0.0542(14) Uani 0.703(6) 1 d P B 1
C13' C 0.4523(4) 0.7305(4) 1.1387(4) 0.059(2) Uani 0.703(6) 1 d P B 1
H13G H 0.5008 0.7621 1.1440 0.088 Uiso 0.703(6) 1 calc PR B 1
H13E H 0.4250 0.7303 1.1976 0.088 Uiso 0.703(6) 1 calc PR B 1
H13F H 0.4183 0.7549 1.0922 0.088 Uiso 0.703(6) 1 calc PR B 1
C7" C 0.6324(12) 0.6123(10) 0.8954(13) 0.024(13) Uiso 0.297(6) 1 d P B 2
C8" C 0.5852(11) 0.6686(11) 0.8729(13) 0.050(6) Uiso 0.297(6) 1 d P B 2
H8" H 0.5940 0.6916 0.8144 0.060 Uiso 0.297(6) 1 calc PR B 2
C9" C 0.5221(11) 0.7016(12) 0.9217(12) 0.063(5) Uiso 0.297(6) 1 d P B 2
H9" H 0.4884 0.7417 0.8967 0.075 Uiso 0.297(6) 1 calc PR B 2
C10" C 0.5137(8) 0.6743(9) 1.0004(10) 0.025(4) Uiso 0.297(6) 1 d P B 2
C11" C 0.5542(8) 0.6078(9) 1.0363(10) 0.027(3) Uiso 0.297(6) 1 d P B 2
H11" H 0.5426 0.5841 1.0938 0.032 Uiso 0.297(6) 1 calc PR B 2
C12" C 0.61516(18) 0.5793(2) 0.9765(2) 0.024(4) Uiso 0.297(6) 1 d PG B 2
H12" H 0.6453 0.5340 0.9958 0.028 Uiso 0.297(6) 1 calc PR B 2
O1" O 0.4491(2) 0.7045(3) 1.0587(4) 0.046(3) Uiso 0.297(6) 1 d PG B 2
C13" C 0.4387(4) 0.6812(4) 1.1519(4) 0.059(5) Uiso 0.297(6) 1 d PG B 2
H13J H 0.4374 0.6220 1.1562 0.089 Uiso 0.297(6) 1 calc PR B 2
H13H H 0.3891 0.7035 1.1749 0.089 Uiso 0.297(6) 1 calc PR B 2
H13I H 0.4825 0.7021 1.1885 0.089 Uiso 0.297(6) 1 calc PR B 2
C1B C 1.1144(2) 0.5043(2) 0.8901(2) 0.0350(9) Uani 1 1 d . . .
O1B O 1.17411(16) 0.47267(15) 0.8834(2) 0.0553(8) Uani 1 1 d . . .
C2B C 0.9680(2) 0.4471(2) 0.8674(2) 0.0281(7) Uani 1 1 d . . .
O2B O 0.94120(15) 0.38929(15) 0.84768(15) 0.0376(6) Uani 1 1 d . . .
B1D B 0.7550(2) 0.5581(2) 0.5127(2) 0.0208(8) Uani 1 1 d . . .
C11D C 0.83709(17) 0.54956(19) 0.45050(19) 0.0205(6) Uani 1 1 d . . .
C12D C 0.8819(2) 0.4825(2) 0.4441(3) 0.0396(9) Uani 1 1 d . . .
H12D H 0.8640 0.4347 0.4737 0.047 Uiso 1 1 calc R . .
C13D C 0.9544(2) 0.4790(2) 0.3958(3) 0.0488(11) Uani 1 1 d . . .
H13D H 0.9831 0.4297 0.3956 0.059 Uiso 1 1 calc R . .
C14D C 0.9836(2) 0.5422(2) 0.3508(2) 0.0313(8) Uani 1 1 d . . .
H14D H 1.0325 0.5400 0.3196 0.038 Uiso 1 1 calc R . .
C15D C 0.9394(2) 0.6092(2) 0.3523(2) 0.0310(8) Uani 1 1 d . . .
H15D H 0.9562 0.6556 0.3194 0.037 Uiso 1 1 calc R . .
C16D C 0.86839(19) 0.6125(2) 0.4019(2) 0.0279(8) Uani 1 1 d . . .
H16D H 0.8402 0.6621 0.4014 0.033 Uiso 1 1 calc R . .
C21D C 0.67547(19) 0.57678(19) 0.4508(2) 0.0256(7) Uani 1 1 d . . .
C22D C 0.6761(2) 0.5948(2) 0.3583(2) 0.0318(8) Uani 1 1 d . . .
H22D H 0.7249 0.5970 0.3267 0.038 Uiso 1 1 calc R . .
C23D C 0.6061(2) 0.6098(2) 0.3104(3) 0.0449(10) Uani 1 1 d . . .
H23D H 0.6085 0.6220 0.2471 0.054 Uiso 1 1 calc R . .
C24D C 0.5326(2) 0.6070(2) 0.3540(3) 0.0462(10) Uani 1 1 d . . .
H24D H 0.4859 0.6176 0.3206 0.055 Uiso 1 1 calc R . .
C25D C 0.5292(2) 0.5891(2) 0.4444(3) 0.0432(10) Uani 1 1 d . . .
H25D H 0.4801 0.5863 0.4750 0.052 Uiso 1 1 calc R . .
C26D C 0.5988(2) 0.5750(2) 0.4913(3) 0.0356(9) Uani 1 1 d . . .
H26D H 0.5954 0.5633 0.5547 0.043 Uiso 1 1 calc R . .
C31D C 0.77146(19) 0.63153(19) 0.5831(2) 0.0246(7) Uani 1 1 d . . .
C32D C 0.7207(2) 0.6958(2) 0.5937(2) 0.0327(8) Uani 1 1 d . . .
H32D H 0.6730 0.6971 0.5600 0.039 Uiso 1 1 calc R . .
C33D C 0.7382(3) 0.7574(2) 0.6520(3) 0.0464(11) Uani 1 1 d . . .
H33D H 0.7030 0.8019 0.6570 0.056 Uiso 1 1 calc R . .
C34D C 0.8061(3) 0.7567(2) 0.7043(2) 0.0480(11) Uani 1 1 d . . .
H34D H 0.8166 0.7998 0.7455 0.058 Uiso 1 1 calc R . .
C35D C 0.8581(2) 0.6938(2) 0.6963(2) 0.0378(9) Uani 1 1 d . . .
H35D H 0.9047 0.6924 0.7320 0.045 Uiso 1 1 calc R . .
C36D C 0.8416(2) 0.6335(2) 0.6364(2) 0.0279(8) Uani 1 1 d . . .
H36D H 0.8784 0.5906 0.6297 0.034 Uiso 1 1 calc R . .
C41D C 0.73738(17) 0.47640(18) 0.5691(2) 0.0198(7) Uani 1 1 d . . .
C42D C 0.76296(19) 0.4608(2) 0.6573(2) 0.0277(7) Uani 1 1 d . . .
H42D H 0.7940 0.5005 0.6874 0.033 Uiso 1 1 calc R . .
C43D C 0.7457(2) 0.3917(2) 0.7021(2) 0.0340(8) Uani 1 1 d . . .
H43D H 0.7639 0.3834 0.7627 0.041 Uiso 1 1 calc R . .
C44D C 0.7019(2) 0.3341(2) 0.6596(2) 0.0332(8) Uani 1 1 d . . .
H44D H 0.6883 0.2857 0.6910 0.040 Uiso 1 1 calc R . .
C45D C 0.67752(19) 0.3458(2) 0.5720(2) 0.0307(8) Uani 1 1 d . . .
H45D H 0.6479 0.3050 0.5419 0.037 Uiso 1 1 calc R . .
C46D C 0.69532(18) 0.4153(2) 0.5278(2) 0.0248(7) Uani 1 1 d . . .
H46D H 0.6783 0.4221 0.4665 0.030 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Rh1 0.03030(15) 0.02016(13) 0.02205(14) -0.00211(12) 0.00508(10) -0.00098(13)
N1 0.0284(16) 0.0241(15) 0.0243(15) -0.0046(12) 0.0019(12) -0.0026(12)
C2 0.0301(19) 0.0245(18) 0.0178(16) -0.0016(13) 0.0015(14) 0.0024(15)
N3 0.0279(15) 0.0241(15) 0.0253(15) -0.0080(12) 0.0014(12) -0.0016(12)
C4 0.032(2) 0.0246(19) 0.038(2) -0.0116(15) -0.0031(17) -0.0032(16)
C5 0.037(2) 0.0259(19) 0.033(2) -0.0090(15) 0.0004(17) -0.0044(16)
C1A 0.0307(19) 0.0296(19) 0.0288(19) -0.0111(15) 0.0062(15) -0.0004(15)
N1' 0.0279(16) 0.0299(16) 0.0255(15) -0.0041(12) 0.0045(12) -0.0057(13)
N2' 0.0299(15) 0.0270(16) 0.0248(14) -0.0036(12) 0.0021(12) -0.0043(13)
N3' 0.0337(16) 0.0220(15) 0.0200(14) -0.0015(11) 0.0048(12) -0.0041(13)
C4' 0.0318(19) 0.0258(18) 0.0225(17) -0.0041(14) 0.0056(15) -0.0063(15)
C5' 0.031(2) 0.0250(18) 0.0271(18) -0.0055(15) 0.0046(15) -0.0024(15)
C6 0.0278(18) 0.0196(17) 0.0286(18) -0.0036(14) 0.0079(15) -0.0044(14)
C7 0.035(2) 0.0253(18) 0.0311(19) -0.0010(15) 0.0027(16) -0.0048(16)
C8 0.036(2) 0.0246(19) 0.046(2) 0.0010(16) 0.0057(18) 0.0021(16)
C9 0.043(2) 0.0218(19) 0.053(2) -0.0122(17) 0.013(2) -0.0062(17)
C10 0.054(3) 0.036(2) 0.032(2) -0.0138(17) 0.0149(19) -0.0112(19)
C11 0.041(2) 0.0283(19) 0.0256(18) -0.0053(15) 0.0040(16) -0.0079(16)
C12 0.042(2) 0.062(3) 0.032(2) 0.0083(19) -0.0029(18) 0.004(2)
C13 0.055(3) 0.047(3) 0.074(3) -0.016(2) 0.031(2) -0.001(2)
C14 0.054(3) 0.064(3) 0.029(2) 0.0010(19) -0.0045(19) -0.008(2)
C6' 0.032(2) 0.041(2) 0.0303(19) -0.0062(16) -0.0029(16) -0.0064(17)
C7' 0.028(7) 0.030(7) 0.031(7) -0.004(2) -0.001(2) -0.003(2)
C8' 0.034(3) 0.027(3) 0.049(4) -0.008(3) 0.003(3) -0.007(3)
C9' 0.035(4) 0.029(3) 0.057(5) -0.004(3) -0.002(3) -0.007(3)
C10' 0.030(3) 0.038(4) 0.030(3) -0.005(3) 0.009(3) -0.005(3)
C11' 0.064(4) 0.029(4) 0.053(4) 0.010(3) 0.020(3) 0.011(3)
C12' 0.065(4) 0.026(3) 0.056(4) 0.003(3) 0.011(3) 0.004(3)
O1' 0.053(3) 0.057(3) 0.053(3) 0.004(2) 0.018(2) 0.014(2)
C13' 0.058(4) 0.074(5) 0.045(4) -0.010(3) 0.012(3) 0.018(4)
C1B 0.045(2) 0.0171(18) 0.043(2) -0.0012(16) 0.0108(18) -0.0020(17)
O1B 0.0413(17) 0.0265(16) 0.098(2) 0.0027(14) 0.0205(16) 0.0057(13)
C2B 0.0360(19) 0.028(2) 0.0203(17) 0.0016(15) 0.0065(15) 0.0021(17)
O2B 0.0566(17) 0.0226(14) 0.0335(14) -0.0030(11) 0.0028(12) -0.0088(13)
B1D 0.0237(19) 0.0174(19) 0.0213(18) 0.0027(14) 0.0012(15) 0.0026(15)
C11D 0.0226(16) 0.0220(16) 0.0170(15) -0.0022(14) -0.0024(13) -0.0010(14)
C12D 0.042(2) 0.0269(19) 0.050(2) 0.0127(17) 0.0235(19) 0.0053(17)
C13D 0.050(2) 0.037(2) 0.060(3) 0.0121(19) 0.032(2) 0.0216(19)
C14D 0.0289(18) 0.042(2) 0.0228(17) 0.0016(17) 0.0067(14) 0.0010(18)
C15D 0.035(2) 0.033(2) 0.0248(18) 0.0065(15) 0.0045(16) -0.0078(17)
C16D 0.034(2) 0.0213(17) 0.0286(18) 0.0030(14) 0.0037(16) 0.0018(15)
C21D 0.0254(18) 0.0169(16) 0.0345(19) 0.0039(14) 0.0008(15) -0.0003(14)
C22D 0.0285(19) 0.030(2) 0.037(2) 0.0067(16) -0.0025(16) -0.0035(16)
C23D 0.043(2) 0.045(2) 0.046(2) 0.0124(19) -0.015(2) -0.0023(19)
C24D 0.033(2) 0.033(2) 0.072(3) 0.010(2) -0.019(2) 0.0006(18)
C25D 0.024(2) 0.035(2) 0.071(3) 0.013(2) 0.0051(19) 0.0052(17)
C26D 0.029(2) 0.030(2) 0.048(2) 0.0089(17) 0.0042(17) 0.0045(16)
C31D 0.0326(19) 0.0195(17) 0.0216(17) 0.0029(13) 0.0123(15) -0.0026(14)
C32D 0.044(2) 0.0272(19) 0.0265(19) 0.0029(15) 0.0079(16) 0.0069(17)
C33D 0.075(3) 0.024(2) 0.039(2) -0.0032(17) 0.023(2) 0.010(2)
C34D 0.082(3) 0.035(2) 0.027(2) -0.0082(17) 0.013(2) -0.015(2)
C35D 0.051(2) 0.038(2) 0.0241(19) -0.0002(16) 0.0072(17) -0.0186(19)
C36D 0.035(2) 0.0263(18) 0.0220(17) 0.0010(14) 0.0085(15) -0.0066(15)
C41D 0.0155(15) 0.0203(17) 0.0236(17) -0.0015(13) 0.0039(13) 0.0049(12)
C42D 0.0342(19) 0.0240(18) 0.0249(17) -0.0019(15) 0.0030(15) 0.0029(16)
C43D 0.048(2) 0.029(2) 0.0247(18) 0.0067(15) 0.0070(17) 0.0051(18)
C44D 0.032(2) 0.0249(19) 0.042(2) 0.0083(16) 0.0180(17) 0.0044(16)
C45D 0.0234(18) 0.0207(18) 0.048(2) -0.0027(16) 0.0027(16) 0.0010(14)
C46D 0.0201(17) 0.0258(18) 0.0285(18) -0.0012(14) -0.0019(14) 0.0045(14)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 C2B 1.860(4) . ?
Rh1 C1B 1.888(4) . ?
Rh1 C2 2.010(3) . ?
Rh1 N3' 2.100(3) . ?
N1 C5 1.333(4) . ?
N1 C2 1.375(4) . ?
N1 C6 1.458(4) . ?
C2 N3 1.352(4) . ?
N3 C4 1.352(4) . ?
N3 C1A 1.484(4) . ?
C4 C5 1.363(5) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C1A C4' 1.471(4) . ?
C1A H1A 0.9900 . ?
C1A H1B 0.9900 . ?
N1' C5' 1.317(4) . ?
N1' N2' 1.331(4) . ?
N1' C6' 1.499(4) . ?
N2' N3' 1.331(4) . ?
N3' C4' 1.327(4) . ?
C4' C5' 1.379(5) . ?
C5' H5' 0.9500 . ?
C6 C11 1.380(4) . ?
C6 C7 1.397(5) . ?
C7 C8 1.406(5) . ?
C7 C12 1.507(5) . ?
C8 C9 1.380(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.399(5) . ?
C9 C13 1.537(5) . ?
C10 C11 1.414(5) . ?
C10 H10 0.9500 . ?
C11 C14 1.516(5) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C6' C7" 1.45(2) . ?
C6' C7' 1.556(4) . ?
C6' H6'1 0.9900 . ?
C6' H6'2 0.9900 . ?
C7' C8' 1.3900 . ?
C7' C12' 1.3900 . ?
C8' C9' 1.3900 . ?
C8' H8' 0.9500 . ?
C9' C10' 1.3900 . ?
C9' H9' 0.9500 . ?
C10' C11' 1.3900 . ?
C10' O1' 1.400(4) . ?
C11' C12' 1.3900 . ?
C11' H11' 0.9500 . ?
C12' H12' 0.9500 . ?
O1' C13' 1.366(7) . ?
C13' H13G 0.9800 . ?
C13' H13E 0.9800 . ?
C13' H13F 0.9800 . ?
C7" C8" 1.27(2) . ?
C7" C12" 1.34(2) . ?
C8" C9" 1.40(2) . ?
C8" H8" 0.9500 . ?
C9" C10" 1.25(2) . ?
C9" H9" 0.9500 . ?
C10" C11" 1.398(19) . ?
C10" O1" 1.479(15) . ?
C11" C12" 1.437(14) . ?
C11" H11" 0.9500 . ?
C12" H12" 0.9500 . ?
O1" C13" 1.4294 . ?
C13" H13J 0.9800 . ?
C13" H13H 0.9800 . ?
C13" H13I 0.9800 . ?
C1B O1B 1.146(4) . ?
C2B O2B 1.097(4) . ?
B1D C41D 1.611(4) . ?
B1D C31D 1.615(5) . ?
B1D C21D 1.658(5) . ?
B1D C11D 1.673(5) . ?
C11D C12D 1.348(5) . ?
C11D C16D 1.368(4) . ?
C12D C13D 1.424(5) . ?
C12D H12D 0.9500 . ?
C13D C14D 1.331(5) . ?
C13D H13D 0.9500 . ?
C14D C15D 1.338(5) . ?
C14D H14D 0.9500 . ?
C15D C16D 1.410(5) . ?
C15D H15D 0.9500 . ?
C16D H16D 0.9500 . ?
C21D C22D 1.387(5) . ?
C21D C26D 1.433(5) . ?
C22D C23D 1.404(5) . ?
C22D H22D 0.9500 . ?
C23D C24D 1.404(5) . ?
C23D H23D 0.9500 . ?
C24D C25D 1.358(5) . ?
C24D H24D 0.9500 . ?
C25D C26D 1.389(5) . ?
C25D H25D 0.9500 . ?
C26D H26D 0.9500 . ?
C31D C32D 1.377(5) . ?
C31D C36D 1.427(5) . ?
C32D C33D 1.362(5) . ?
C32D H32D 0.9500 . ?
C33D C34D 1.386(6) . ?
C33D H33D 0.9500 . ?
C34D C35D 1.369(5) . ?
C34D H34D 0.9500 . ?
C35D C36D 1.358(5) . ?
C35D H35D 0.9500 . ?
C36D H36D 0.9500 . ?
C41D C46D 1.378(4) . ?
C41D C42D 1.387(4) . ?
C42D C43D 1.350(5) . ?
C42D H42D 0.9500 . ?
C43D C44D 1.360(5) . ?
C43D H43D 0.9500 . ?
C44D C45D 1.362(5) . ?
C44D H44D 0.9500 . ?
C45D C46D 1.353(5) . ?
C45D H45D 0.9500 . ?
C46D H46D 0.9500 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2B Rh1 C1B 91.51(15) . . ?
C2B Rh1 C2 175.44(14) . . ?
C1B Rh1 C2 92.47(14) . . ?
C2B Rh1 N3' 87.23(13) . . ?
C1B Rh1 N3' 176.76(13) . . ?
C2 Rh1 N3' 88.68(12) . . ?
C5 N1 C2 109.6(3) . . ?
C5 N1 C6 120.7(3) . . ?
C2 N1 C6 129.7(3) . . ?
N3 C2 N1 106.5(3) . . ?
N3 C2 Rh1 122.3(2) . . ?
N1 C2 Rh1 131.1(2) . . ?
C4 N3 C2 108.3(3) . . ?
C4 N3 C1A 123.7(3) . . ?
C2 N3 C1A 127.9(3) . . ?
N3 C4 C5 108.7(3) . . ?
N3 C4 H4 125.7 . . ?
C5 C4 H4 125.7 . . ?
N1 C5 C4 107.0(3) . . ?
N1 C5 H5 126.5 . . ?
C4 C5 H5 126.5 . . ?
C4' C1A N3 114.0(3) . . ?
C4' C1A H1A 108.8 . . ?
N3 C1A H1A 108.8 . . ?
C4' C1A H1B 108.8 . . ?
N3 C1A H1B 108.8 . . ?
H1A C1A H1B 107.7 . . ?
C5' N1' N2' 110.5(3) . . ?
C5' N1' C6' 126.9(3) . . ?
N2' N1' C6' 122.6(3) . . ?
N3' N2' N1' 107.6(2) . . ?
C4' N3' N2' 108.2(3) . . ?
C4' N3' Rh1 127.5(2) . . ?
N2' N3' Rh1 124.2(2) . . ?
N3' C4' C5' 108.2(3) . . ?
N3' C4' C1A 120.5(3) . . ?
C5' C4' C1A 131.0(3) . . ?
N1' C5' C4' 105.5(3) . . ?
N1' C5' H5' 127.2 . . ?
C4' C5' H5' 127.2 . . ?
C11 C6 C7 122.0(3) . . ?
C11 C6 N1 118.4(3) . . ?
C7 C6 N1 119.4(3) . . ?
C6 C7 C8 118.4(3) . . ?
C6 C7 C12 120.5(3) . . ?
C8 C7 C12 121.1(3) . . ?
C9 C8 C7 122.4(3) . . ?
C9 C8 H8 118.8 . . ?
C7 C8 H8 118.8 . . ?
C8 C9 C10 116.8(3) . . ?
C8 C9 C13 120.5(4) . . ?
C10 C9 C13 122.6(4) . . ?
C9 C10 C11 123.3(3) . . ?
C9 C10 H10 118.4 . . ?
C11 C10 H10 118.4 . . ?
C6 C11 C10 117.1(3) . . ?
C6 C11 C14 120.6(3) . . ?
C10 C11 C14 122.2(3) . . ?
C7 C12 H12A 109.5 . . ?
C7 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C7 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C9 C13 H13A 109.5 . . ?
C9 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C9 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C7" C6' N1' 110.6(7) . . ?
C7" C6' C7' 2.5(8) . . ?
N1' C6' C7' 111.1(3) . . ?
C7" C6' H6'1 111.8 . . ?
N1' C6' H6'1 109.4 . . ?
C7' C6' H6'1 109.4 . . ?
C7" C6' H6'2 107.5 . . ?
N1' C6' H6'2 109.4 . . ?
C7' C6' H6'2 109.4 . . ?
H6'1 C6' H6'2 108.0 . . ?
C8' C7' C12' 120.0 . . ?
C8' C7' C6' 122.2(3) . . ?
C12' C7' C6' 117.3(3) . . ?
C7' C8' C9' 120.0 . . ?
C7' C8' H8' 120.0 . . ?
C9' C8' H8' 120.0 . . ?
C10' C9' C8' 120.0 . . ?
C10' C9' H9' 120.0 . . ?
C8' C9' H9' 120.0 . . ?
C9' C10' C11' 120.0 . . ?
C9' C10' O1' 126.1(3) . . ?
C11' C10' O1' 113.9(3) . . ?
C12' C11' C10' 120.0 . . ?
C12' C11' H11' 120.0 . . ?
C10' C11' H11' 120.0 . . ?
C11' C12' C7' 120.0 . . ?
C11' C12' H12' 120.0 . . ?
C7' C12' H12' 120.0 . . ?
C13' O1' C10' 116.6(5) . . ?
C8" C7" C12" 112.9(18) . . ?
C8" C7" C6' 118.5(18) . . ?
C12" C7" C6' 128.6(11) . . ?
C7" C8" C9" 130(2) . . ?
C7" C8" H8" 115.2 . . ?
C9" C8" H8" 115.2 . . ?
C10" C9" C8" 114.8(18) . . ?
C10" C9" H9" 122.6 . . ?
C8" C9" H9" 122.6 . . ?
C9" C10" C11" 125.1(15) . . ?
C9" C10" O1" 119.8(14) . . ?
C11" C10" O1" 114.5(10) . . ?
C10" C11" C12" 112.6(11) . . ?
C10" C11" H11" 123.7 . . ?
C12" C11" H11" 123.7 . . ?
C7" C12" C11" 124.4(9) . . ?
C7" C12" H12" 117.8 . . ?
C11" C12" H12" 117.8 . . ?
C13" O1" C10" 123.5(5) . . ?
O1" C13" H13J 109.5 . . ?
O1" C13" H13H 109.5 . . ?
H13J C13" H13H 109.5 . . ?
O1" C13" H13I 109.5 . . ?
H13J C13" H13I 109.5 . . ?
H13H C13" H13I 109.5 . . ?
O1B C1B Rh1 174.2(3) . . ?
O2B C2B Rh1 178.9(3) . . ?
C41D B1D C31D 109.6(2) . . ?
C41D B1D C21D 106.5(3) . . ?
C31D B1D C21D 110.5(3) . . ?
C41D B1D C11D 111.3(3) . . ?
C31D B1D C11D 105.4(2) . . ?
C21D B1D C11D 113.5(2) . . ?
C12D C11D C16D 111.6(3) . . ?
C12D C11D B1D 125.4(3) . . ?
C16D C11D B1D 123.0(3) . . ?
C11D C12D C13D 123.9(3) . . ?
C11D C12D H12D 118.0 . . ?
C13D C12D H12D 118.0 . . ?
C14D C13D C12D 122.5(3) . . ?
C14D C13D H13D 118.8 . . ?
C12D C13D H13D 118.8 . . ?
C13D C14D C15D 115.6(3) . . ?
C13D C14D H14D 122.2 . . ?
C15D C14D H14D 122.2 . . ?
C14D C15D C16D 121.4(3) . . ?
C14D C15D H15D 119.3 . . ?
C16D C15D H15D 119.3 . . ?
C11D C16D C15D 124.9(3) . . ?
C11D C16D H16D 117.5 . . ?
C15D C16D H16D 117.5 . . ?
C22D C21D C26D 114.6(3) . . ?
C22D C21D B1D 124.6(3) . . ?
C26D C21D B1D 120.8(3) . . ?
C21D C22D C23D 121.2(3) . . ?
C21D C22D H22D 119.4 . . ?
C23D C22D H22D 119.4 . . ?
C24D C23D C22D 121.5(4) . . ?
C24D C23D H23D 119.2 . . ?
C22D C23D H23D 119.2 . . ?
C25D C24D C23D 119.2(3) . . ?
C25D C24D H24D 120.4 . . ?
C23D C24D H24D 120.4 . . ?
C24D C25D C26D 118.8(4) . . ?
C24D C25D H25D 120.6 . . ?
C26D C25D H25D 120.6 . . ?
C25D C26D C21D 124.6(3) . . ?
C25D C26D H26D 117.7 . . ?
C21D C26D H26D 117.7 . . ?
C32D C31D C36D 116.4(3) . . ?
C32D C31D B1D 122.8(3) . . ?
C36D C31D B1D 120.7(3) . . ?
C33D C32D C31D 120.7(4) . . ?
C33D C32D H32D 119.6 . . ?
C31D C32D H32D 119.6 . . ?
C32D C33D C34D 121.5(4) . . ?
C32D C33D H33D 119.3 . . ?
C34D C33D H33D 119.3 . . ?
C35D C34D C33D 119.8(4) . . ?
C35D C34D H34D 120.1 . . ?
C33D C34D H34D 120.1 . . ?
C36D C35D C34D 118.7(4) . . ?
C36D C35D H35D 120.7 . . ?
C34D C35D H35D 120.7 . . ?
C35D C36D C31D 122.9(3) . . ?
C35D C36D H36D 118.6 . . ?
C31D C36D H36D 118.6 . . ?
C46D C41D C42D 115.9(3) . . ?
C46D C41D B1D 119.1(3) . . ?
C42D C41D B1D 125.1(3) . . ?
C43D C42D C41D 122.8(3) . . ?
C43D C42D H42D 118.6 . . ?
C41D C42D H42D 118.6 . . ?
C42D C43D C44D 119.3(3) . . ?
C42D C43D H43D 120.4 . . ?
C44D C43D H43D 120.4 . . ?
C43D C44D C45D 119.9(3) . . ?
C43D C44D H44D 120.0 . . ?
C45D C44D H44D 120.0 . . ?
C46D C45D C44D 120.3(3) . . ?
C46D C45D H45D 119.9 . . ?
C44D C45D H45D 119.9 . . ?
C45D C46D C41D 121.9(3) . . ?
C45D C46D H46D 119.1 . . ?
C41D C46D H46D 119.1 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 C2 N3 -0.3(3) . . . . ?
C6 N1 C2 N3 -178.6(3) . . . . ?
C5 N1 C2 Rh1 177.1(2) . . . . ?
C6 N1 C2 Rh1 -1.2(5) . . . . ?
C2B Rh1 C2 N3 47.5(17) . . . . ?
C1B Rh1 C2 N3 -161.7(3) . . . . ?
N3' Rh1 C2 N3 21.3(2) . . . . ?
C2B Rh1 C2 N1 -129.6(16) . . . . ?
C1B Rh1 C2 N1 21.2(3) . . . . ?
N3' Rh1 C2 N1 -155.8(3) . . . . ?
N1 C2 N3 C4 -0.2(3) . . . . ?
Rh1 C2 N3 C4 -177.9(2) . . . . ?
N1 C2 N3 C1A -176.3(3) . . . . ?
Rh1 C2 N3 C1A 6.0(4) . . . . ?
C2 N3 C4 C5 0.7(4) . . . . ?
C1A N3 C4 C5 176.9(3) . . . . ?
C2 N1 C5 C4 0.7(4) . . . . ?
C6 N1 C5 C4 179.2(3) . . . . ?
N3 C4 C5 N1 -0.8(4) . . . . ?
C4 N3 C1A C4' 140.2(3) . . . . ?
C2 N3 C1A C4' -44.3(4) . . . . ?
C5' N1' N2' N3' 0.4(3) . . . . ?
C6' N1' N2' N3' 178.3(3) . . . . ?
N1' N2' N3' C4' 0.0(3) . . . . ?
N1' N2' N3' Rh1 -176.19(19) . . . . ?
C2B Rh1 N3' C4' 161.2(3) . . . . ?
C1B Rh1 N3' C4' -132(2) . . . . ?
C2 Rh1 N3' C4' -20.8(3) . . . . ?
C2B Rh1 N3' N2' -23.4(2) . . . . ?
C1B Rh1 N3' N2' 44(2) . . . . ?
C2 Rh1 N3' N2' 154.6(2) . . . . ?
N2' N3' C4' C5' -0.5(4) . . . . ?
Rh1 N3' C4' C5' 175.6(2) . . . . ?
N2' N3' C4' C1A 175.2(3) . . . . ?
Rh1 N3' C4' C1A -8.7(4) . . . . ?
N3 C1A C4' N3' 43.4(4) . . . . ?
N3 C1A C4' C5' -142.0(3) . . . . ?
N2' N1' C5' C4' -0.7(4) . . . . ?
C6' N1' C5' C4' -178.5(3) . . . . ?
N3' C4' C5' N1' 0.7(4) . . . . ?
C1A C4' C5' N1' -174.4(3) . . . . ?
C5 N1 C6 C11 -98.7(4) . . . . ?
C2 N1 C6 C11 79.4(4) . . . . ?
C5 N1 C6 C7 76.2(4) . . . . ?
C2 N1 C6 C7 -105.6(4) . . . . ?
C11 C6 C7 C8 0.2(5) . . . . ?
N1 C6 C7 C8 -174.6(3) . . . . ?
C11 C6 C7 C12 -179.4(3) . . . . ?
N1 C6 C7 C12 5.8(5) . . . . ?
C6 C7 C8 C9 -0.3(5) . . . . ?
C12 C7 C8 C9 179.3(3) . . . . ?
C7 C8 C9 C10 -0.7(5) . . . . ?
C7 C8 C9 C13 178.9(3) . . . . ?
C8 C9 C10 C11 1.8(5) . . . . ?
C13 C9 C10 C11 -177.8(3) . . . . ?
C7 C6 C11 C10 0.8(5) . . . . ?
N1 C6 C11 C10 175.7(3) . . . . ?
C7 C6 C11 C14 -175.7(3) . . . . ?
N1 C6 C11 C14 -0.9(5) . . . . ?
C9 C10 C11 C6 -1.9(5) . . . . ?
C9 C10 C11 C14 174.6(4) . . . . ?
C5' N1' C6' C7" -38.2(9) . . . . ?
N2' N1' C6' C7" 144.2(8) . . . . ?
C5' N1' C6' C7' -40.9(5) . . . . ?
N2' N1' C6' C7' 141.6(3) . . . . ?
C7" C6' C7' C8' 14(17) . . . . ?
N1' C6' C7' C8' 92.9(3) . . . . ?
C7" C6' C7' C12' -159(18) . . . . ?
N1' C6' C7' C12' -79.2(4) . . . . ?
C12' C7' C8' C9' 0.0 . . . . ?
C6' C7' C8' C9' -172.0(4) . . . . ?
C7' C8' C9' C10' 0.0 . . . . ?
C8' C9' C10' C11' 0.0 . . . . ?
C8' C9' C10' O1' 178.0(4) . . . . ?
C9' C10' C11' C12' 0.0 . . . . ?
O1' C10' C11' C12' -178.3(3) . . . . ?
C10' C11' C12' C7' 0.0 . . . . ?
C8' C7' C12' C11' 0.0 . . . . ?
C6' C7' C12' C11' 172.3(4) . . . . ?
C9' C10' O1' C13' -18.7(6) . . . . ?
C11' C10' O1' C13' 159.5(4) . . . . ?
N1' C6' C7" C8" 117.3(15) . . . . ?
C7' C6' C7" C8" -141(18) . . . . ?
N1' C6' C7" C12" -63.5(19) . . . . ?
C7' C6' C7" C12" 38(16) . . . . ?
C12" C7" C8" C9" 3(3) . . . . ?
C6' C7" C8" C9" -177.7(16) . . . . ?
C7" C8" C9" C10" 4(3) . . . . ?
C8" C9" C10" C11" -9(2) . . . . ?
C8" C9" C10" O1" 180.0(13) . . . . ?
C9" C10" C11" C12" 8(2) . . . . ?
O1" C10" C11" C12" 178.6(9) . . . . ?
C8" C7" C12" C11" -5(2) . . . . ?
C6' C7" C12" C11" 176.0(12) . . . . ?
C10" C11" C12" C7" 0.3(18) . . . . ?
C9" C10" O1" C13" -175.1(11) . . . . ?
C11" C10" O1" C13" 13.4(14) . . . . ?
C2B Rh1 C1B O1B -18(3) . . . . ?
C2 Rh1 C1B O1B 164(3) . . . . ?
N3' Rh1 C1B O1B -85(4) . . . . ?
C1B Rh1 C2B O2B 163(17) . . . . ?
C2 Rh1 C2B O2B -46(17) . . . . ?
N3' Rh1 C2B O2B -20(17) . . . . ?
C41D B1D C11D C12D 2.6(4) . . . . ?
C31D B1D C11D C12D 121.4(3) . . . . ?
C21D B1D C11D C12D -117.5(4) . . . . ?
C41D B1D C11D C16D -174.9(3) . . . . ?
C31D B1D C11D C16D -56.1(4) . . . . ?
C21D B1D C11D C16D 65.0(4) . . . . ?
C16D C11D C12D C13D 2.4(5) . . . . ?
B1D C11D C12D C13D -175.3(3) . . . . ?
C11D C12D C13D C14D -1.4(7) . . . . ?
C12D C13D C14D C15D -1.2(6) . . . . ?
C13D C14D C15D C16D 2.4(5) . . . . ?
C12D C11D C16D C15D -1.2(5) . . . . ?
B1D C11D C16D C15D 176.6(3) . . . . ?
C14D C15D C16D C11D -1.3(5) . . . . ?
C41D B1D C21D C22D -131.3(3) . . . . ?
C31D B1D C21D C22D 109.8(4) . . . . ?
C11D B1D C21D C22D -8.4(4) . . . . ?
C41D B1D C21D C26D 48.6(4) . . . . ?
C31D B1D C21D C26D -70.3(4) . . . . ?
C11D B1D C21D C26D 171.4(3) . . . . ?
C26D C21D C22D C23D 0.0(5) . . . . ?
B1D C21D C22D C23D 179.9(3) . . . . ?
C21D C22D C23D C24D -0.1(6) . . . . ?
C22D C23D C24D C25D -0.3(6) . . . . ?
C23D C24D C25D C26D 0.8(6) . . . . ?
C24D C25D C26D C21D -0.9(6) . . . . ?
C22D C21D C26D C25D 0.5(5) . . . . ?
B1D C21D C26D C25D -179.4(3) . . . . ?
C41D B1D C31D C32D -111.5(3) . . . . ?
C21D B1D C31D C32D 5.6(4) . . . . ?
C11D B1D C31D C32D 128.6(3) . . . . ?
C41D B1D C31D C36D 70.0(4) . . . . ?
C21D B1D C31D C36D -172.9(3) . . . . ?
C11D B1D C31D C36D -49.9(4) . . . . ?
C36D C31D C32D C33D 0.4(5) . . . . ?
B1D C31D C32D C33D -178.1(3) . . . . ?
C31D C32D C33D C34D -1.8(6) . . . . ?
C32D C33D C34D C35D 1.4(6) . . . . ?
C33D C34D C35D C36D 0.4(5) . . . . ?
C34D C35D C36D C31D -1.8(5) . . . . ?
C32D C31D C36D C35D 1.3(5) . . . . ?
B1D C31D C36D C35D 180.0(3) . . . . ?
C31D B1D C41D C46D 156.9(3) . . . . ?
C21D B1D C41D C46D 37.3(4) . . . . ?
C11D B1D C41D C46D -86.9(3) . . . . ?
C31D B1D C41D C42D -24.6(4) . . . . ?
C21D B1D C41D C42D -144.2(3) . . . . ?
C11D B1D C41D C42D 91.6(3) . . . . ?
C46D C41D C42D C43D -2.5(5) . . . . ?
B1D C41D C42D C43D 179.0(3) . . . . ?
C41D C42D C43D C44D 0.5(5) . . . . ?
C42D C43D C44D C45D 1.5(5) . . . . ?
C43D C44D C45D C46D -1.4(5) . . . . ?
C44D C45D C46D C41D -0.7(5) . . . . ?
C42D C41D C46D C45D 2.5(5) . . . . ?
B1D C41D C46D C45D -178.9(3) . . . . ?
_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max 0.314
_refine_diff_density_min -0.366
_refine_diff_density_rms 0.069
_database_code_depnum_ccdc_archive 'CCDC 934039'
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_platon
#TrackingRef 'Khuong8_Deposition_30May12.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C30 H36 N6 Rh, C24 H20 B'
_chemical_formula_sum 'C54 H56 B N6 Rh'
_chemical_formula_weight 902.77
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Triclinic
_symmetry_space_group_name_H-M P-1
_symmetry_space_group_name_Hall '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 11.0540(4)
_cell_length_b 15.1556(6)
_cell_length_c 15.2020(6)
_cell_angle_alpha 112.774(2)
_cell_angle_beta 102.466(2)
_cell_angle_gamma 90.891(2)
_cell_volume 2278.94(15)
_cell_formula_units_Z 2
_cell_measurement_temperature 150(2)
_cell_measurement_reflns_used 8861
_cell_measurement_theta_min 2.342
_cell_measurement_theta_max 24.164
_exptl_crystal_description 'Thin Plates'
_exptl_crystal_colour Yellow
_exptl_crystal_size_max 0.43
_exptl_crystal_size_mid 0.17
_exptl_crystal_size_min 0.07
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.316
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 944
_exptl_absorpt_coefficient_mu 0.419
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.8421
_exptl_absorpt_correction_T_max 0.9717
_exptl_absorpt_process_details 'SADABS (Bruker, 2001)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 150(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker kappa APEXII CCD Diffractometer'
_diffrn_measurement_method '\f scans, and \w scans with \k offsets'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 31905
_diffrn_reflns_av_R_equivalents 0.0540
_diffrn_reflns_av_sigmaI/netI 0.0555
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_theta_min 2.52
_diffrn_reflns_theta_max 25.00
_reflns_number_total 7968
_reflns_number_gt 6463
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2007)'
_computing_cell_refinement 'APEX2 (Bruker, 2007)'
_computing_data_reduction 'APEX2 (Bruker, 2007)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
Atoms of One of the phenyl rings (C21-C26) of the anion (BPh4) exhibited high thermal anisotropies, therefore the six atoms were constrained to a regular six membered ring using command AFIX 66 in SHELXL.
The NH2 groups make short N-H...N type interactions, this gives the alert level B
PLAT417_ALERT_2_B Short Inter D-H..H-D H4'2 .. H4'2 ..1.95 Ang.
Although not common, such short contacts are reported.
K.-L. Park, B.-G. Moon, S.-H. Jung, J.-G. Kim and I.-H. Suh
Acta Cryst. (2000). C56, 1247-1250.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0379P)^2^+1.8478P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 7968
_refine_ls_number_parameters 550
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0535
_refine_ls_R_factor_gt 0.0361
_refine_ls_wR_factor_ref 0.0899
_refine_ls_wR_factor_gt 0.0815
_refine_ls_goodness_of_fit_ref 1.016
_refine_ls_restrained_S_all 1.016
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C21C C 0.30302(19) 0.32930(11) 0.73092(14) 0.0244(7) Uani 1 1 d G . .
C22C C 0.23202(19) 0.24279(14) 0.66694(13) 0.0388(9) Uani 1 1 d G . .
H22C H 0.1704 0.2408 0.6136 0.047 Uiso 1 1 calc R . .
C23C C 0.2532(2) 0.15933(11) 0.68272(16) 0.0561(12) Uani 1 1 d G . .
H23C H 0.2057 0.1015 0.6399 0.067 Uiso 1 1 calc R . .
C24C C 0.3453(3) 0.16238(14) 0.76248(19) 0.0638(14) Uani 1 1 d G . .
H24C H 0.3595 0.1065 0.7730 0.077 Uiso 1 1 calc R . .
C25C C 0.4164(2) 0.24889(19) 0.82646(16) 0.0504(11) Uani 1 1 d G . .
H25C H 0.4780 0.2509 0.8798 0.061 Uiso 1 1 calc R . .
C26C C 0.39519(18) 0.33235(14) 0.81068(13) 0.0345(8) Uani 1 1 d G . .
H26C H 0.4427 0.3902 0.8535 0.041 Uiso 1 1 calc R . .
Rh1 Rh 0.77794(2) 0.141106(16) 0.686869(16) 0.02000(8) Uani 1 1 d . . .
N1 N 0.8287(2) 0.28308(16) 0.91052(16) 0.0203(5) Uani 1 1 d . . .
C2 C 0.7724(3) 0.2557(2) 0.8132(2) 0.0205(6) Uani 1 1 d . . .
N3 N 0.7095(2) 0.33110(17) 0.81191(16) 0.0228(6) Uani 1 1 d . . .
C4 C 0.7248(3) 0.4030(2) 0.9045(2) 0.0259(7) Uani 1 1 d . . .
H4 H 0.6896 0.4608 0.9206 0.031 Uiso 1 1 calc R . .
C5 C 0.8003(3) 0.3733(2) 0.9667(2) 0.0255(7) Uani 1 1 d . . .
H5 H 0.8282 0.4067 1.0344 0.031 Uiso 1 1 calc R . .
C1A C 0.6319(3) 0.3346(2) 0.7220(2) 0.0298(7) Uani 1 1 d . . .
H1A1 H 0.6025 0.3976 0.7373 0.036 Uiso 1 1 calc R . .
H1A2 H 0.5597 0.2871 0.6973 0.036 Uiso 1 1 calc R . .
N1' N 0.7805(2) 0.30678(17) 0.52399(18) 0.0280(6) Uani 1 1 d . . .
N2' N 0.8215(2) 0.23577(17) 0.54938(18) 0.0270(6) Uani 1 1 d . . .
N3' N 0.7727(2) 0.24096(17) 0.62289(16) 0.0230(6) Uani 1 1 d . . .
C4' C 0.7026(3) 0.3155(2) 0.6446(2) 0.0226(6) Uani 1 1 d . . .
C5' C 0.7072(3) 0.3574(2) 0.5803(2) 0.0306(7) Uani 1 1 d . . .
H5' H 0.6678 0.4100 0.5765 0.037 Uiso 1 1 calc R . .
C6 C 0.9154(3) 0.23118(19) 0.95217(19) 0.0200(6) Uani 1 1 d . . .
C7 C 0.8765(3) 0.1845(2) 1.00592(19) 0.0228(7) Uani 1 1 d . . .
C8 C 0.9654(3) 0.1396(2) 1.0495(2) 0.0289(7) Uani 1 1 d . . .
H8 H 0.9419 0.1083 1.0860 0.035 Uiso 1 1 calc R . .
C9 C 1.0863(3) 0.1401(2) 1.0402(2) 0.0276(7) Uani 1 1 d . . .
C10 C 1.1196(3) 0.1849(2) 0.9834(2) 0.0274(7) Uani 1 1 d . . .
H10 H 1.2002 0.1830 0.9742 0.033 Uiso 1 1 calc R . .
C11 C 1.0368(3) 0.2324(2) 0.9398(2) 0.0241(7) Uani 1 1 d . . .
C12 C 0.7452(3) 0.1828(2) 1.0179(2) 0.0343(8) Uani 1 1 d . . .
H12A H 0.7334 0.1401 1.0491 0.052 Uiso 1 1 calc R . .
H12B H 0.6879 0.1608 0.9545 0.052 Uiso 1 1 calc R . .
H12C H 0.7303 0.2465 1.0578 0.052 Uiso 1 1 calc R . .
C13 C 1.1829(3) 0.0962(2) 1.0932(3) 0.0423(9) Uani 1 1 d . . .
H13A H 1.2359 0.0638 1.0511 0.063 Uiso 1 1 calc R . .
H13B H 1.1418 0.0510 1.1102 0.063 Uiso 1 1 calc R . .
H13C H 1.2323 0.1462 1.1520 0.063 Uiso 1 1 calc R . .
C14 C 1.0763(3) 0.2834(2) 0.8824(2) 0.0356(8) Uani 1 1 d . . .
H14A H 1.1645 0.2832 0.8885 0.053 Uiso 1 1 calc R . .
H14B H 1.0565 0.3487 0.9075 0.053 Uiso 1 1 calc R . .
H14C H 1.0332 0.2513 0.8145 0.053 Uiso 1 1 calc R . .
C6' C 0.8128(3) 0.3161(2) 0.4383(2) 0.0340(8) Uani 1 1 d . . .
H6'1 H 0.9027 0.3205 0.4474 0.041 Uiso 1 1 calc R . .
H6'2 H 0.7851 0.3749 0.4336 0.041 Uiso 1 1 calc R . .
C7' C 0.7534(3) 0.2316(2) 0.3445(2) 0.0285(7) Uani 1 1 d . . .
C8' C 0.8160(3) 0.1516(2) 0.3111(2) 0.0382(8) Uani 1 1 d . . .
H8' H 0.8967 0.1520 0.3455 0.046 Uiso 1 1 calc R . .
C9' C 0.7615(4) 0.0712(3) 0.2281(2) 0.0438(9) Uani 1 1 d . . .
H9' H 0.8061 0.0186 0.2071 0.053 Uiso 1 1 calc R . .
C10' C 0.6419(3) 0.0678(3) 0.1758(2) 0.0390(9) Uani 1 1 d . . .
C11' C 0.5796(3) 0.1480(3) 0.2076(3) 0.0456(9) Uani 1 1 d . . .
H11' H 0.4993 0.1475 0.1724 0.055 Uiso 1 1 calc R . .
C12' C 0.6334(3) 0.2287(3) 0.2901(3) 0.0431(9) Uani 1 1 d . . .
H12' H 0.5893 0.2819 0.3098 0.052 Uiso 1 1 calc R . .
N4' N 0.5878(3) -0.0136(2) 0.0903(2) 0.0586(9) Uani 1 1 d . . .
H4'1 H 0.6294 -0.0620 0.0701 0.070 Uiso 1 1 calc R . .
H4'2 H 0.5130 -0.0152 0.0580 0.070 Uiso 1 1 calc R . .
C1B C 0.8147(3) 0.0347(2) 0.7477(2) 0.0257(7) Uani 1 1 d . . .
H1B H 0.8652 0.0835 0.8027 0.031 Uiso 1 1 calc R . .
C2B C 0.6878(3) 0.0429(2) 0.7281(2) 0.0251(7) Uani 1 1 d . . .
H2B H 0.6594 0.0944 0.7732 0.030 Uiso 1 1 calc R . .
C3B C 0.5919(3) -0.0253(2) 0.6391(2) 0.0313(7) Uani 1 1 d . . .
H3B1 H 0.5167 0.0059 0.6315 0.038 Uiso 1 1 calc R . .
H3B2 H 0.5709 -0.0819 0.6502 0.038 Uiso 1 1 calc R . .
C4B C 0.6360(3) -0.0572(2) 0.5438(2) 0.0300(7) Uani 1 1 d . . .
H4B1 H 0.6825 -0.1121 0.5376 0.036 Uiso 1 1 calc R . .
H4B2 H 0.5639 -0.0774 0.4884 0.036 Uiso 1 1 calc R . .
C5B C 0.7170(3) 0.0218(2) 0.5400(2) 0.0267(7) Uani 1 1 d . . .
H5B H 0.6772 0.0651 0.5172 0.032 Uiso 1 1 calc R . .
C6B C 0.8448(3) 0.0346(2) 0.5678(2) 0.0254(7) Uani 1 1 d . . .
H6B H 0.8847 0.0849 0.5604 0.030 Uiso 1 1 calc R . .
C7B C 0.9257(3) -0.0259(2) 0.6092(2) 0.0326(8) Uani 1 1 d . . .
H7B1 H 1.0094 0.0072 0.6381 0.039 Uiso 1 1 calc R . .
H7B2 H 0.9301 -0.0864 0.5560 0.039 Uiso 1 1 calc R . .
C8B C 0.8775(3) -0.0470(2) 0.6871(2) 0.0295(7) Uani 1 1 d . . .
H8B1 H 0.8187 -0.1047 0.6549 0.035 Uiso 1 1 calc R . .
H8B2 H 0.9469 -0.0595 0.7306 0.035 Uiso 1 1 calc R . .
B1C B 0.2806(3) 0.4267(2) 0.7029(2) 0.0211(7) Uani 1 1 d . . .
C11C C 0.1657(3) 0.4813(2) 0.74413(19) 0.0215(6) Uani 1 1 d . . .
C12C C 0.1542(3) 0.5777(2) 0.7594(2) 0.0240(7) Uani 1 1 d . . .
H12D H 0.2167 0.6119 0.7494 0.029 Uiso 1 1 calc R . .
C13C C 0.0547(3) 0.6243(2) 0.7887(2) 0.0324(8) Uani 1 1 d . . .
H13D H 0.0498 0.6879 0.7963 0.039 Uiso 1 1 calc R . .
C14C C -0.0374(3) 0.5764(3) 0.8068(2) 0.0383(9) Uani 1 1 d . . .
H14D H -0.1038 0.6079 0.8282 0.046 Uiso 1 1 calc R . .
C15C C -0.0307(3) 0.4817(3) 0.7930(2) 0.0390(9) Uani 1 1 d . . .
H15C H -0.0925 0.4488 0.8052 0.047 Uiso 1 1 calc R . .
C16C C 0.0685(3) 0.4353(2) 0.7610(2) 0.0291(7) Uani 1 1 d . . .
H16C H 0.0702 0.3706 0.7503 0.035 Uiso 1 1 calc R . .
C31C C 0.4060(3) 0.5051(2) 0.7498(2) 0.0233(7) Uani 1 1 d . . .
C32C C 0.4480(3) 0.5580(2) 0.8513(2) 0.0388(8) Uani 1 1 d . . .
H32C H 0.4020 0.5496 0.8926 0.047 Uiso 1 1 calc R . .
C33C C 0.5558(4) 0.6225(3) 0.8928(3) 0.0553(11) Uani 1 1 d . . .
H33C H 0.5815 0.6552 0.9607 0.066 Uiso 1 1 calc R . .
C34C C 0.6249(3) 0.6384(3) 0.8334(3) 0.0528(11) Uani 1 1 d . . .
H34C H 0.6971 0.6813 0.8608 0.063 Uiso 1 1 calc R . .
C35C C 0.5851(3) 0.5899(2) 0.7340(3) 0.0455(10) Uani 1 1 d . . .
H35C H 0.6302 0.6002 0.6931 0.055 Uiso 1 1 calc R . .
C36C C 0.4775(3) 0.5253(2) 0.6933(2) 0.0295(7) Uani 1 1 d . . .
H36C H 0.4520 0.4941 0.6252 0.035 Uiso 1 1 calc R . .
C41C C 0.2477(3) 0.38950(19) 0.5823(2) 0.0201(6) Uani 1 1 d . . .
C42C C 0.3198(3) 0.3265(2) 0.5260(2) 0.0245(7) Uani 1 1 d . . .
H42C H 0.3855 0.3039 0.5579 0.029 Uiso 1 1 calc R . .
C43C C 0.2976(3) 0.2963(2) 0.4250(2) 0.0276(7) Uani 1 1 d . . .
H43C H 0.3481 0.2546 0.3907 0.033 Uiso 1 1 calc R . .
C44C C 0.1999(3) 0.3284(2) 0.3752(2) 0.0305(8) Uani 1 1 d . . .
H44C H 0.1831 0.3075 0.3072 0.037 Uiso 1 1 calc R . .
C45C C 0.1284(3) 0.3915(2) 0.4281(2) 0.0314(8) Uani 1 1 d . . .
H45C H 0.0640 0.4149 0.3958 0.038 Uiso 1 1 calc R . .
C46C C 0.1516(3) 0.4207(2) 0.5292(2) 0.0257(7) Uani 1 1 d . . .
H46C H 0.1011 0.4629 0.5629 0.031 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C21C 0.0278(17) 0.0292(17) 0.0221(15) 0.0114(13) 0.0152(13) 0.0081(13)
C22C 0.068(3) 0.0263(18) 0.0248(16) 0.0099(14) 0.0181(17) 0.0021(17)
C23C 0.113(4) 0.028(2) 0.041(2) 0.0155(18) 0.046(2) 0.008(2)
C24C 0.109(4) 0.055(3) 0.081(3) 0.056(3) 0.073(3) 0.052(3)
C25C 0.050(2) 0.078(3) 0.061(3) 0.056(2) 0.034(2) 0.035(2)
C26C 0.0319(19) 0.049(2) 0.0374(19) 0.0286(17) 0.0154(15) 0.0125(16)
Rh1 0.02260(14) 0.01946(13) 0.01685(12) 0.00663(9) 0.00368(9) 0.00329(9)
N1 0.0193(13) 0.0229(13) 0.0171(12) 0.0074(10) 0.0022(10) 0.0033(10)
C2 0.0186(16) 0.0240(16) 0.0205(15) 0.0116(13) 0.0028(12) 0.0026(13)
N3 0.0220(14) 0.0271(14) 0.0198(12) 0.0105(11) 0.0034(10) 0.0079(11)
C4 0.0261(17) 0.0250(16) 0.0265(16) 0.0068(14) 0.0120(13) 0.0108(13)
C5 0.0283(18) 0.0235(16) 0.0218(15) 0.0048(13) 0.0081(13) 0.0057(13)
C1A 0.0279(18) 0.043(2) 0.0285(17) 0.0224(15) 0.0094(14) 0.0192(15)
N1' 0.0375(16) 0.0240(14) 0.0282(14) 0.0129(12) 0.0141(12) 0.0070(12)
N2' 0.0317(15) 0.0262(14) 0.0269(14) 0.0120(12) 0.0116(12) 0.0058(12)
N3' 0.0261(14) 0.0256(14) 0.0198(12) 0.0108(11) 0.0072(11) 0.0037(11)
C4' 0.0222(16) 0.0246(16) 0.0224(15) 0.0101(13) 0.0061(13) 0.0091(13)
C5' 0.039(2) 0.0275(17) 0.0293(17) 0.0134(15) 0.0127(15) 0.0129(15)
C6 0.0235(17) 0.0175(15) 0.0130(13) 0.0024(11) -0.0006(12) 0.0029(12)
C7 0.0253(17) 0.0226(16) 0.0149(14) 0.0034(12) 0.0016(12) -0.0020(13)
C8 0.041(2) 0.0225(16) 0.0204(15) 0.0091(13) 0.0012(14) -0.0036(14)
C9 0.0325(19) 0.0180(15) 0.0236(16) 0.0054(13) -0.0052(14) 0.0017(13)
C10 0.0257(18) 0.0228(16) 0.0257(16) 0.0042(13) 0.0005(13) 0.0035(13)
C11 0.0254(17) 0.0223(16) 0.0207(15) 0.0060(13) 0.0026(13) 0.0016(13)
C12 0.035(2) 0.040(2) 0.0285(17) 0.0143(15) 0.0074(15) -0.0031(16)
C13 0.049(2) 0.0332(19) 0.038(2) 0.0163(16) -0.0072(17) 0.0074(17)
C14 0.0265(19) 0.046(2) 0.043(2) 0.0259(17) 0.0100(15) 0.0080(15)
C6' 0.047(2) 0.0297(18) 0.0359(18) 0.0197(15) 0.0196(16) 0.0063(16)
C7' 0.037(2) 0.0302(18) 0.0304(17) 0.0210(15) 0.0151(15) 0.0087(15)
C8' 0.036(2) 0.043(2) 0.0335(18) 0.0147(17) 0.0043(16) 0.0168(17)
C9' 0.057(3) 0.040(2) 0.0329(19) 0.0136(17) 0.0082(18) 0.0215(18)
C10' 0.047(2) 0.045(2) 0.0309(18) 0.0243(17) 0.0040(17) -0.0015(18)
C11' 0.028(2) 0.064(3) 0.047(2) 0.029(2) 0.0023(17) 0.0086(19)
C12' 0.040(2) 0.050(2) 0.055(2) 0.032(2) 0.0221(19) 0.0249(18)
N4' 0.071(2) 0.059(2) 0.0346(17) 0.0165(16) -0.0057(16) -0.0045(18)
C1B 0.037(2) 0.0188(16) 0.0190(15) 0.0080(13) 0.0020(13) 0.0005(14)
C2B 0.0314(19) 0.0207(16) 0.0266(16) 0.0107(13) 0.0113(14) 0.0058(13)
C3B 0.0283(18) 0.0275(17) 0.0361(18) 0.0128(15) 0.0039(14) -0.0011(14)
C4B 0.0293(18) 0.0262(17) 0.0254(16) 0.0057(14) -0.0030(14) 0.0013(14)
C5B 0.0316(19) 0.0238(16) 0.0210(15) 0.0075(13) 0.0016(13) 0.0061(14)
C6B 0.0285(18) 0.0231(16) 0.0242(15) 0.0077(13) 0.0089(13) 0.0059(13)
C7B 0.0316(19) 0.0298(18) 0.0330(18) 0.0076(15) 0.0098(15) 0.0123(14)
C8B 0.0311(19) 0.0216(16) 0.0318(17) 0.0098(14) 0.0010(14) 0.0062(14)
B1C 0.0225(19) 0.0228(18) 0.0171(16) 0.0073(14) 0.0042(14) 0.0006(14)
C11C 0.0223(16) 0.0259(16) 0.0130(13) 0.0074(12) -0.0012(12) -0.0008(13)
C12C 0.0245(17) 0.0254(16) 0.0177(14) 0.0063(13) 0.0008(12) 0.0027(13)
C13C 0.038(2) 0.0340(19) 0.0153(15) 0.0026(14) 0.0002(14) 0.0129(16)
C14C 0.0262(19) 0.063(3) 0.0194(16) 0.0095(16) 0.0046(14) 0.0174(17)
C15C 0.0236(19) 0.066(3) 0.0270(17) 0.0176(17) 0.0063(14) -0.0026(17)
C16C 0.0294(18) 0.0335(18) 0.0242(16) 0.0117(14) 0.0065(14) -0.0010(15)
C31C 0.0187(16) 0.0177(15) 0.0286(16) 0.0065(13) 0.0009(13) 0.0064(12)
C32C 0.0274(19) 0.040(2) 0.0340(18) 0.0011(16) 0.0030(15) 0.0055(16)
C33C 0.037(2) 0.040(2) 0.052(2) -0.0123(19) -0.0047(19) 0.0019(18)
C34C 0.023(2) 0.027(2) 0.082(3) -0.002(2) 0.005(2) -0.0032(16)
C35C 0.031(2) 0.0270(19) 0.077(3) 0.016(2) 0.0199(19) 0.0028(16)
C36C 0.0267(18) 0.0201(16) 0.0421(19) 0.0118(14) 0.0100(15) 0.0041(13)
C41C 0.0215(16) 0.0188(15) 0.0224(15) 0.0106(12) 0.0060(12) -0.0001(12)
C42C 0.0248(17) 0.0261(16) 0.0262(16) 0.0141(13) 0.0061(13) 0.0040(13)
C43C 0.0357(19) 0.0244(16) 0.0244(16) 0.0076(13) 0.0147(14) 0.0054(14)
C44C 0.040(2) 0.0327(18) 0.0184(15) 0.0096(14) 0.0074(14) -0.0014(15)
C45C 0.0306(19) 0.042(2) 0.0227(16) 0.0153(15) 0.0030(14) 0.0061(15)
C46C 0.0259(17) 0.0292(17) 0.0225(15) 0.0099(13) 0.0077(13) 0.0050(13)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C21C C22C 1.3900 . ?
C21C C26C 1.3900 . ?
C21C B1C 1.695(4) . ?
C22C C23C 1.3900 . ?
C22C H22C 0.9300 . ?
C23C C24C 1.3900 . ?
C23C H23C 0.9300 . ?
C24C C25C 1.3900 . ?
C24C H24C 0.9300 . ?
C25C C26C 1.3900 . ?
C25C H25C 0.9300 . ?
C26C H26C 0.9300 . ?
Rh1 C2 2.045(3) . ?
Rh1 N3' 2.087(2) . ?
Rh1 C2B 2.132(3) . ?
Rh1 C1B 2.153(3) . ?
Rh1 C6B 2.186(3) . ?
Rh1 C5B 2.212(3) . ?
N1 C2 1.366(3) . ?
N1 C5 1.387(4) . ?
N1 C6 1.445(3) . ?
C2 N3 1.351(4) . ?
N3 C4 1.379(4) . ?
N3 C1A 1.469(3) . ?
C4 C5 1.339(4) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C1A C4' 1.490(4) . ?
C1A H1A1 0.9700 . ?
C1A H1A2 0.9700 . ?
N1' N2' 1.332(3) . ?
N1' C5' 1.337(4) . ?
N1' C6' 1.479(4) . ?
N2' N3' 1.319(3) . ?
N3' C4' 1.354(4) . ?
C4' C5' 1.364(4) . ?
C5' H5' 0.9300 . ?
C6 C7 1.395(4) . ?
C6 C11 1.395(4) . ?
C7 C8 1.398(4) . ?
C7 C12 1.503(4) . ?
C8 C9 1.373(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.389(4) . ?
C9 C13 1.516(4) . ?
C10 C11 1.387(4) . ?
C10 H10 0.9300 . ?
C11 C14 1.491(4) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C6' C7' 1.503(4) . ?
C6' H6'1 0.9700 . ?
C6' H6'2 0.9700 . ?
C7' C8' 1.381(4) . ?
C7' C12' 1.393(5) . ?
C8' C9' 1.378(5) . ?
C8' H8' 0.9300 . ?
C9' C10' 1.376(5) . ?
C9' H9' 0.9300 . ?
C10' C11' 1.378(5) . ?
C10' N4' 1.404(4) . ?
C11' C12' 1.376(5) . ?
C11' H11' 0.9300 . ?
C12' H12' 0.9300 . ?
N4' H4'1 0.8600 . ?
N4' H4'2 0.8600 . ?
C1B C2B 1.388(4) . ?
C1B C8B 1.511(4) . ?
C1B H1B 0.9300 . ?
C2B C3B 1.512(4) . ?
C2B H2B 0.9300 . ?
C3B C4B 1.530(4) . ?
C3B H3B1 0.9700 . ?
C3B H3B2 0.9700 . ?
C4B C5B 1.509(4) . ?
C4B H4B1 0.9700 . ?
C4B H4B2 0.9700 . ?
C5B C6B 1.372(4) . ?
C5B H5B 0.9300 . ?
C6B C7B 1.505(4) . ?
C6B H6B 0.9300 . ?
C7B C8B 1.534(4) . ?
C7B H7B1 0.9700 . ?
C7B H7B2 0.9700 . ?
C8B H8B1 0.9700 . ?
C8B H8B2 0.9700 . ?
B1C C11C 1.632(5) . ?
B1C C31C 1.646(4) . ?
B1C C41C 1.648(4) . ?
C11C C16C 1.393(4) . ?
C11C C12C 1.400(4) . ?
C12C C13C 1.378(4) . ?
C12C H12D 0.9300 . ?
C13C C14C 1.375(5) . ?
C13C H13D 0.9300 . ?
C14C C15C 1.373(5) . ?
C14C H14D 0.9300 . ?
C15C C16C 1.388(5) . ?
C15C H15C 0.9300 . ?
C16C H16C 0.9300 . ?
C31C C36C 1.395(4) . ?
C31C C32C 1.400(4) . ?
C32C C33C 1.392(5) . ?
C32C H32C 0.9300 . ?
C33C C34C 1.385(6) . ?
C33C H33C 0.9300 . ?
C34C C35C 1.364(5) . ?
C34C H34C 0.9300 . ?
C35C C36C 1.390(4) . ?
C35C H35C 0.9300 . ?
C36C H36C 0.9300 . ?
C41C C46C 1.395(4) . ?
C41C C42C 1.402(4) . ?
C42C C43C 1.384(4) . ?
C42C H42C 0.9300 . ?
C43C C44C 1.387(4) . ?
C43C H43C 0.9300 . ?
C44C C45C 1.374(5) . ?
C44C H44C 0.9300 . ?
C45C C46C 1.387(4) . ?
C45C H45C 0.9300 . ?
C46C H46C 0.9300 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C22C C21C C26C 120.0 . . ?
C22C C21C B1C 117.77(16) . . ?
C26C C21C B1C 122.06(16) . . ?
C21C C22C C23C 120.0 . . ?
C21C C22C H22C 120.0 . . ?
C23C C22C H22C 120.0 . . ?
C22C C23C C24C 120.0 . . ?
C22C C23C H23C 120.0 . . ?
C24C C23C H23C 120.0 . . ?
C25C C24C C23C 120.0 . . ?
C25C C24C H24C 120.0 . . ?
C23C C24C H24C 120.0 . . ?
C26C C25C C24C 120.0 . . ?
C26C C25C H25C 120.0 . . ?
C24C C25C H25C 120.0 . . ?
C25C C26C C21C 120.0 . . ?
C25C C26C H26C 120.0 . . ?
C21C C26C H26C 120.0 . . ?
C2 Rh1 N3' 85.87(10) . . ?
C2 Rh1 C2B 92.50(11) . . ?
N3' Rh1 C2B 151.47(11) . . ?
C2 Rh1 C1B 98.37(11) . . ?
N3' Rh1 C1B 170.11(11) . . ?
C2B Rh1 C1B 37.79(11) . . ?
C2 Rh1 C6B 162.34(11) . . ?
N3' Rh1 C6B 91.99(10) . . ?
C2B Rh1 C6B 97.60(12) . . ?
C1B Rh1 C6B 81.25(11) . . ?
C2 Rh1 C5B 160.93(11) . . ?
N3' Rh1 C5B 90.68(10) . . ?
C2B Rh1 C5B 81.64(11) . . ?
C1B Rh1 C5B 88.11(11) . . ?
C6B Rh1 C5B 36.34(11) . . ?
C2 N1 C5 111.4(2) . . ?
C2 N1 C6 126.2(2) . . ?
C5 N1 C6 122.3(2) . . ?
N3 C2 N1 103.2(2) . . ?
N3 C2 Rh1 121.90(19) . . ?
N1 C2 Rh1 134.7(2) . . ?
C2 N3 C4 112.2(2) . . ?
C2 N3 C1A 123.5(2) . . ?
C4 N3 C1A 124.2(2) . . ?
C5 C4 N3 106.6(3) . . ?
C5 C4 H4 126.7 . . ?
N3 C4 H4 126.7 . . ?
C4 C5 N1 106.6(3) . . ?
C4 C5 H5 126.7 . . ?
N1 C5 H5 126.7 . . ?
N3 C1A C4' 111.5(2) . . ?
N3 C1A H1A1 109.3 . . ?
C4' C1A H1A1 109.3 . . ?
N3 C1A H1A2 109.3 . . ?
C4' C1A H1A2 109.3 . . ?
H1A1 C1A H1A2 108.0 . . ?
N2' N1' C5' 111.6(2) . . ?
N2' N1' C6' 118.9(3) . . ?
C5' N1' C6' 129.3(3) . . ?
N3' N2' N1' 105.9(2) . . ?
N2' N3' C4' 110.0(2) . . ?
N2' N3' Rh1 126.75(19) . . ?
C4' N3' Rh1 122.72(19) . . ?
N3' C4' C5' 107.1(3) . . ?
N3' C4' C1A 121.0(2) . . ?
C5' C4' C1A 131.8(3) . . ?
N1' C5' C4' 105.4(3) . . ?
N1' C5' H5' 127.3 . . ?
C4' C5' H5' 127.3 . . ?
C7 C6 C11 122.4(3) . . ?
C7 C6 N1 119.1(3) . . ?
C11 C6 N1 118.5(2) . . ?
C6 C7 C8 117.1(3) . . ?
C6 C7 C12 121.9(3) . . ?
C8 C7 C12 121.0(3) . . ?
C9 C8 C7 122.4(3) . . ?
C9 C8 H8 118.8 . . ?
C7 C8 H8 118.8 . . ?
C8 C9 C10 118.3(3) . . ?
C8 C9 C13 121.4(3) . . ?
C10 C9 C13 120.3(3) . . ?
C11 C10 C9 122.3(3) . . ?
C11 C10 H10 118.9 . . ?
C9 C10 H10 118.9 . . ?
C10 C11 C6 117.5(3) . . ?
C10 C11 C14 121.3(3) . . ?
C6 C11 C14 121.3(3) . . ?
C7 C12 H12A 109.5 . . ?
C7 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C7 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C9 C13 H13A 109.5 . . ?
C9 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C9 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N1' C6' C7' 111.2(2) . . ?
N1' C6' H6'1 109.4 . . ?
C7' C6' H6'1 109.4 . . ?
N1' C6' H6'2 109.4 . . ?
C7' C6' H6'2 109.4 . . ?
H6'1 C6' H6'2 108.0 . . ?
C8' C7' C12' 117.5(3) . . ?
C8' C7' C6' 120.1(3) . . ?
C12' C7' C6' 122.3(3) . . ?
C9' C8' C7' 121.5(3) . . ?
C9' C8' H8' 119.3 . . ?
C7' C8' H8' 119.3 . . ?
C10' C9' C8' 120.9(3) . . ?
C10' C9' H9' 119.6 . . ?
C8' C9' H9' 119.6 . . ?
C9' C10' C11' 118.0(3) . . ?
C9' C10' N4' 120.6(4) . . ?
C11' C10' N4' 121.3(3) . . ?
C12' C11' C10' 121.5(3) . . ?
C12' C11' H11' 119.3 . . ?
C10' C11' H11' 119.3 . . ?
C11' C12' C7' 120.6(3) . . ?
C11' C12' H12' 119.7 . . ?
C7' C12' H12' 119.7 . . ?
C10' N4' H4'1 120.0 . . ?
C10' N4' H4'2 120.0 . . ?
H4'1 N4' H4'2 120.0 . . ?
C2B C1B C8B 125.4(3) . . ?
C2B C1B Rh1 70.31(16) . . ?
C8B C1B Rh1 112.86(19) . . ?
C2B C1B H1B 117.3 . . ?
C8B C1B H1B 117.3 . . ?
Rh1 C1B H1B 86.8 . . ?
C1B C2B C3B 125.2(3) . . ?
C1B C2B Rh1 71.90(17) . . ?
C3B C2B Rh1 108.63(19) . . ?
C1B C2B H2B 117.4 . . ?
C3B C2B H2B 117.4 . . ?
Rh1 C2B H2B 89.5 . . ?
C2B C3B C4B 113.5(3) . . ?
C2B C3B H3B1 108.9 . . ?
C4B C3B H3B1 108.9 . . ?
C2B C3B H3B2 108.9 . . ?
C4B C3B H3B2 108.9 . . ?
H3B1 C3B H3B2 107.7 . . ?
C5B C4B C3B 112.5(2) . . ?
C5B C4B H4B1 109.1 . . ?
C3B C4B H4B1 109.1 . . ?
C5B C4B H4B2 109.1 . . ?
C3B C4B H4B2 109.1 . . ?
H4B1 C4B H4B2 107.8 . . ?
C6B C5B C4B 125.1(3) . . ?
C6B C5B Rh1 70.80(17) . . ?
C4B C5B Rh1 110.81(19) . . ?
C6B C5B H5B 117.5 . . ?
C4B C5B H5B 117.5 . . ?
Rh1 C5B H5B 88.4 . . ?
C5B C6B C7B 125.4(3) . . ?
C5B C6B Rh1 72.86(18) . . ?
C7B C6B Rh1 108.32(19) . . ?
C5B C6B H6B 117.3 . . ?
C7B C6B H6B 117.3 . . ?
Rh1 C6B H6B 88.8 . . ?
C6B C7B C8B 113.0(3) . . ?
C6B C7B H7B1 109.0 . . ?
C8B C7B H7B1 109.0 . . ?
C6B C7B H7B2 109.0 . . ?
C8B C7B H7B2 109.0 . . ?
H7B1 C7B H7B2 107.8 . . ?
C1B C8B C7B 112.9(2) . . ?
C1B C8B H8B1 109.0 . . ?
C7B C8B H8B1 109.0 . . ?
C1B C8B H8B2 109.0 . . ?
C7B C8B H8B2 109.0 . . ?
H8B1 C8B H8B2 107.8 . . ?
C11C B1C C31C 108.0(2) . . ?
C11C B1C C41C 109.3(2) . . ?
C31C B1C C41C 108.4(2) . . ?
C11C B1C C21C 111.2(2) . . ?
C31C B1C C21C 111.8(2) . . ?
C41C B1C C21C 108.1(2) . . ?
C16C C11C C12C 114.9(3) . . ?
C16C C11C B1C 123.3(3) . . ?
C12C C11C B1C 121.7(3) . . ?
C13C C12C C11C 123.1(3) . . ?
C13C C12C H12D 118.5 . . ?
C11C C12C H12D 118.5 . . ?
C14C C13C C12C 119.8(3) . . ?
C14C C13C H13D 120.1 . . ?
C12C C13C H13D 120.1 . . ?
C15C C14C C13C 119.5(3) . . ?
C15C C14C H14D 120.3 . . ?
C13C C14C H14D 120.3 . . ?
C14C C15C C16C 119.8(3) . . ?
C14C C15C H15C 120.1 . . ?
C16C C15C H15C 120.1 . . ?
C15C C16C C11C 122.8(3) . . ?
C15C C16C H16C 118.6 . . ?
C11C C16C H16C 118.6 . . ?
C36C C31C C32C 114.8(3) . . ?
C36C C31C B1C 123.6(3) . . ?
C32C C31C B1C 121.5(3) . . ?
C33C C32C C31C 122.5(4) . . ?
C33C C32C H32C 118.7 . . ?
C31C C32C H32C 118.7 . . ?
C34C C33C C32C 120.3(4) . . ?
C34C C33C H33C 119.9 . . ?
C32C C33C H33C 119.9 . . ?
C35C C34C C33C 118.8(3) . . ?
C35C C34C H34C 120.6 . . ?
C33C C34C H34C 120.6 . . ?
C34C C35C C36C 120.5(4) . . ?
C34C C35C H35C 119.8 . . ?
C36C C35C H35C 119.8 . . ?
C35C C36C C31C 123.0(3) . . ?
C35C C36C H36C 118.5 . . ?
C31C C36C H36C 118.5 . . ?
C46C C41C C42C 115.0(3) . . ?
C46C C41C B1C 123.5(3) . . ?
C42C C41C B1C 121.4(3) . . ?
C43C C42C C41C 123.0(3) . . ?
C43C C42C H42C 118.5 . . ?
C41C C42C H42C 118.5 . . ?
C42C C43C C44C 119.9(3) . . ?
C42C C43C H43C 120.1 . . ?
C44C C43C H43C 120.1 . . ?
C45C C44C C43C 118.8(3) . . ?
C45C C44C H44C 120.6 . . ?
C43C C44C H44C 120.6 . . ?
C44C C45C C46C 120.6(3) . . ?
C44C C45C H45C 119.7 . . ?
C46C C45C H45C 119.7 . . ?
C45C C46C C41C 122.7(3) . . ?
C45C C46C H46C 118.7 . . ?
C41C C46C H46C 118.7 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C26C C21C C22C C23C 0.0 . . . . ?
B1C C21C C22C C23C 175.4(2) . . . . ?
C21C C22C C23C C24C 0.0 . . . . ?
C22C C23C C24C C25C 0.0 . . . . ?
C23C C24C C25C C26C 0.0 . . . . ?
C24C C25C C26C C21C 0.0 . . . . ?
C22C C21C C26C C25C 0.0 . . . . ?
B1C C21C C26C C25C -175.1(2) . . . . ?
C5 N1 C2 N3 -0.1(3) . . . . ?
C6 N1 C2 N3 -175.2(2) . . . . ?
C5 N1 C2 Rh1 174.9(2) . . . . ?
C6 N1 C2 Rh1 -0.2(4) . . . . ?
N3' Rh1 C2 N3 33.4(2) . . . . ?
C2B Rh1 C2 N3 -118.1(2) . . . . ?
C1B Rh1 C2 N3 -155.6(2) . . . . ?
C6B Rh1 C2 N3 117.0(4) . . . . ?
C5B Rh1 C2 N3 -46.7(4) . . . . ?
N3' Rh1 C2 N1 -140.9(3) . . . . ?
C2B Rh1 C2 N1 67.7(3) . . . . ?
C1B Rh1 C2 N1 30.1(3) . . . . ?
C6B Rh1 C2 N1 -57.3(5) . . . . ?
C5B Rh1 C2 N1 139.1(3) . . . . ?
N1 C2 N3 C4 -0.2(3) . . . . ?
Rh1 C2 N3 C4 -176.03(19) . . . . ?
N1 C2 N3 C1A -179.2(2) . . . . ?
Rh1 C2 N3 C1A 5.0(4) . . . . ?
C2 N3 C4 C5 0.5(3) . . . . ?
C1A N3 C4 C5 179.4(3) . . . . ?
N3 C4 C5 N1 -0.5(3) . . . . ?
C2 N1 C5 C4 0.4(3) . . . . ?
C6 N1 C5 C4 175.7(3) . . . . ?
C2 N3 C1A C4' -53.4(4) . . . . ?
C4 N3 C1A C4' 127.8(3) . . . . ?
C5' N1' N2' N3' 0.4(3) . . . . ?
C6' N1' N2' N3' -176.1(2) . . . . ?
N1' N2' N3' C4' -0.8(3) . . . . ?
N1' N2' N3' Rh1 171.25(18) . . . . ?
C2 Rh1 N3' N2' 150.5(2) . . . . ?
C2B Rh1 N3' N2' -121.9(3) . . . . ?
C1B Rh1 N3' N2' 34.6(7) . . . . ?
C6B Rh1 N3' N2' -12.0(2) . . . . ?
C5B Rh1 N3' N2' -48.3(2) . . . . ?
C2 Rh1 N3' C4' -38.4(2) . . . . ?
C2B Rh1 N3' C4' 49.2(3) . . . . ?
C1B Rh1 N3' C4' -154.3(5) . . . . ?
C6B Rh1 N3' C4' 159.2(2) . . . . ?
C5B Rh1 N3' C4' 122.8(2) . . . . ?
N2' N3' C4' C5' 0.9(3) . . . . ?
Rh1 N3' C4' C5' -171.55(19) . . . . ?
N2' N3' C4' C1A 177.1(3) . . . . ?
Rh1 N3' C4' C1A 4.6(4) . . . . ?
N3 C1A C4' N3' 46.7(4) . . . . ?
N3 C1A C4' C5' -138.2(3) . . . . ?
N2' N1' C5' C4' 0.1(3) . . . . ?
C6' N1' C5' C4' 176.1(3) . . . . ?
N3' C4' C5' N1' -0.6(3) . . . . ?
C1A C4' C5' N1' -176.2(3) . . . . ?
C2 N1 C6 C7 -107.9(3) . . . . ?
C5 N1 C6 C7 77.5(3) . . . . ?
C2 N1 C6 C11 74.2(4) . . . . ?
C5 N1 C6 C11 -100.4(3) . . . . ?
C11 C6 C7 C8 1.3(4) . . . . ?
N1 C6 C7 C8 -176.6(2) . . . . ?
C11 C6 C7 C12 -179.4(3) . . . . ?
N1 C6 C7 C12 2.8(4) . . . . ?
C6 C7 C8 C9 -0.4(4) . . . . ?
C12 C7 C8 C9 -179.7(3) . . . . ?
C7 C8 C9 C10 -1.7(4) . . . . ?
C7 C8 C9 C13 176.2(3) . . . . ?
C8 C9 C10 C11 2.9(4) . . . . ?
C13 C9 C10 C11 -175.0(3) . . . . ?
C9 C10 C11 C6 -2.1(4) . . . . ?
C9 C10 C11 C14 177.4(3) . . . . ?
C7 C6 C11 C10 -0.1(4) . . . . ?
N1 C6 C11 C10 177.8(2) . . . . ?
C7 C6 C11 C14 -179.6(3) . . . . ?
N1 C6 C11 C14 -1.8(4) . . . . ?
N2' N1' C6' C7' 65.7(4) . . . . ?
C5' N1' C6' C7' -110.1(4) . . . . ?
N1' C6' C7' C8' -90.7(4) . . . . ?
N1' C6' C7' C12' 87.0(4) . . . . ?
C12' C7' C8' C9' -1.0(5) . . . . ?
C6' C7' C8' C9' 176.8(3) . . . . ?
C7' C8' C9' C10' -0.4(5) . . . . ?
C8' C9' C10' C11' 1.6(5) . . . . ?
C8' C9' C10' N4' 178.8(3) . . . . ?
C9' C10' C11' C12' -1.3(5) . . . . ?
N4' C10' C11' C12' -178.5(3) . . . . ?
C10' C11' C12' C7' -0.2(5) . . . . ?
C8' C7' C12' C11' 1.3(5) . . . . ?
C6' C7' C12' C11' -176.4(3) . . . . ?
C2 Rh1 C1B C2B 83.22(18) . . . . ?
N3' Rh1 C1B C2B -161.9(5) . . . . ?
C6B Rh1 C1B C2B -114.63(19) . . . . ?
C5B Rh1 C1B C2B -78.76(18) . . . . ?
C2 Rh1 C1B C8B -155.7(2) . . . . ?
N3' Rh1 C1B C8B -40.8(7) . . . . ?
C2B Rh1 C1B C8B 121.1(3) . . . . ?
C6B Rh1 C1B C8B 6.5(2) . . . . ?
C5B Rh1 C1B C8B 42.3(2) . . . . ?
C8B C1B C2B C3B -4.2(5) . . . . ?
Rh1 C1B C2B C3B 100.4(3) . . . . ?
C8B C1B C2B Rh1 -104.6(3) . . . . ?
C2 Rh1 C2B C1B -100.47(18) . . . . ?
N3' Rh1 C2B C1B 173.58(19) . . . . ?
C6B Rh1 C2B C1B 65.01(18) . . . . ?
C5B Rh1 C2B C1B 97.77(18) . . . . ?
C2 Rh1 C2B C3B 137.5(2) . . . . ?
N3' Rh1 C2B C3B 51.6(3) . . . . ?
C1B Rh1 C2B C3B -122.0(3) . . . . ?
C6B Rh1 C2B C3B -57.0(2) . . . . ?
C5B Rh1 C2B C3B -24.2(2) . . . . ?
C1B C2B C3B C4B -40.9(4) . . . . ?
Rh1 C2B C3B C4B 39.7(3) . . . . ?
C2B C3B C4B C5B -35.7(4) . . . . ?
C3B C4B C5B C6B 94.2(4) . . . . ?
C3B C4B C5B Rh1 13.6(3) . . . . ?
C2 Rh1 C5B C6B 171.7(3) . . . . ?
N3' Rh1 C5B C6B 92.43(18) . . . . ?
C2B Rh1 C5B C6B -115.16(19) . . . . ?
C1B Rh1 C5B C6B -77.75(19) . . . . ?
C2 Rh1 C5B C4B -67.1(4) . . . . ?
N3' Rh1 C5B C4B -146.3(2) . . . . ?
C2B Rh1 C5B C4B 6.1(2) . . . . ?
C1B Rh1 C5B C4B 43.5(2) . . . . ?
C6B Rh1 C5B C4B 121.2(3) . . . . ?
C4B C5B C6B C7B -1.8(5) . . . . ?
Rh1 C5B C6B C7B 100.6(3) . . . . ?
C4B C5B C6B Rh1 -102.4(3) . . . . ?
C2 Rh1 C6B C5B -171.1(3) . . . . ?
N3' Rh1 C6B C5B -88.45(18) . . . . ?
C2B Rh1 C6B C5B 64.61(19) . . . . ?
C1B Rh1 C6B C5B 98.80(19) . . . . ?
C2 Rh1 C6B C7B 66.5(4) . . . . ?
N3' Rh1 C6B C7B 149.1(2) . . . . ?
C2B Rh1 C6B C7B -57.9(2) . . . . ?
C1B Rh1 C6B C7B -23.7(2) . . . . ?
C5B Rh1 C6B C7B -122.5(3) . . . . ?
C5B C6B C7B C8B -44.2(4) . . . . ?
Rh1 C6B C7B C8B 37.5(3) . . . . ?
C2B C1B C8B C7B 93.5(4) . . . . ?
Rh1 C1B C8B C7B 12.1(3) . . . . ?
C6B C7B C8B C1B -33.5(4) . . . . ?
C22C C21C B1C C11C 85.8(2) . . . . ?
C26C C21C B1C C11C -98.9(2) . . . . ?
C22C C21C B1C C31C -153.39(19) . . . . ?
C26C C21C B1C C31C 21.9(3) . . . . ?
C22C C21C B1C C41C -34.1(3) . . . . ?
C26C C21C B1C C41C 141.10(19) . . . . ?
C31C B1C C11C C16C -148.2(3) . . . . ?
C41C B1C C11C C16C 94.0(3) . . . . ?
C21C B1C C11C C16C -25.2(4) . . . . ?
C31C B1C C11C C12C 35.8(3) . . . . ?
C41C B1C C11C C12C -82.0(3) . . . . ?
C21C B1C C11C C12C 158.8(2) . . . . ?
C16C C11C C12C C13C -0.1(4) . . . . ?
B1C C11C C12C C13C 176.2(3) . . . . ?
C11C C12C C13C C14C 1.8(4) . . . . ?
C12C C13C C14C C15C -1.6(4) . . . . ?
C13C C14C C15C C16C -0.1(5) . . . . ?
C14C C15C C16C C11C 1.8(5) . . . . ?
C12C C11C C16C C15C -1.7(4) . . . . ?
B1C C11C C16C C15C -177.9(3) . . . . ?
C11C B1C C31C C36C -125.4(3) . . . . ?
C41C B1C C31C C36C -7.0(4) . . . . ?
C21C B1C C31C C36C 112.0(3) . . . . ?
C11C B1C C31C C32C 53.9(4) . . . . ?
C41C B1C C31C C32C 172.2(3) . . . . ?
C21C B1C C31C C32C -68.7(4) . . . . ?
C36C C31C C32C C33C -2.7(5) . . . . ?
B1C C31C C32C C33C 178.0(3) . . . . ?
C31C C32C C33C C34C 1.5(6) . . . . ?
C32C C33C C34C C35C 0.2(6) . . . . ?
C33C C34C C35C C36C -0.4(6) . . . . ?
C34C C35C C36C C31C -1.0(5) . . . . ?
C32C C31C C36C C35C 2.5(5) . . . . ?
B1C C31C C36C C35C -178.3(3) . . . . ?
C11C B1C C41C C46C 13.9(4) . . . . ?
C31C B1C C41C C46C -103.7(3) . . . . ?
C21C B1C C41C C46C 135.0(3) . . . . ?
C11C B1C C41C C42C -169.1(2) . . . . ?
C31C B1C C41C C42C 73.3(3) . . . . ?
C21C B1C C41C C42C -48.0(3) . . . . ?
C46C C41C C42C C43C -0.5(4) . . . . ?
B1C C41C C42C C43C -177.8(3) . . . . ?
C41C C42C C43C C44C -0.3(4) . . . . ?
C42C C43C C44C C45C 1.3(4) . . . . ?
C43C C44C C45C C46C -1.6(5) . . . . ?
C44C C45C C46C C41C 0.8(5) . . . . ?
C42C C41C C46C C45C 0.2(4) . . . . ?
B1C C41C C46C C45C 177.4(3) . . . . ?
_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max 0.734
_refine_diff_density_min -0.651
_refine_diff_density_rms 0.076
_database_code_depnum_ccdc_archive 'CCDC 934040'
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_inp21byn
#TrackingRef 'Khuong_2_Deposition_11May12.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C22 H23 N6 O2, C24 H20 B'
_chemical_formula_sum 'C46 H43 B N6 O2'
_chemical_formula_weight 722.67
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M P2(1)/n
_symmetry_space_group_name_Hall '-P 2yn '
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 20.119(3)
_cell_length_b 9.3929(13)
_cell_length_c 21.433(4)
_cell_angle_alpha 90.00
_cell_angle_beta 105.532(6)
_cell_angle_gamma 90.00
_cell_volume 3902.4(11)
_cell_formula_units_Z 4
_cell_measurement_temperature 150(2)
_cell_measurement_reflns_used 834
_cell_measurement_theta_min 2.495
_cell_measurement_theta_max 17.722
_exptl_crystal_description Plates
_exptl_crystal_colour Yellow
_exptl_crystal_size_max 0.16
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.03
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.230
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1528
_exptl_absorpt_coefficient_mu 0.076
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.9877
_exptl_absorpt_correction_T_max 0.9976
_exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 150(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker kappa APEXII CCD Area Detector'
_diffrn_measurement_method '\f scans, and \w scans with \k offsets'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 28144
_diffrn_reflns_av_R_equivalents 0.2193
_diffrn_reflns_av_sigmaI/netI 0.2537
_diffrn_reflns_limit_h_min -23
_diffrn_reflns_limit_h_max 23
_diffrn_reflns_limit_k_min -8
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_l_min -25
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_theta_min 2.47
_diffrn_reflns_theta_max 25.00
_reflns_number_total 6864
_reflns_number_gt 2578
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2007)'
_computing_cell_refinement 'APEX2 (Bruker, 2007)'
_computing_data_reduction 'APEX2 (Bruker, 2007)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
Crystals were thin plates and diffracted weakly, which has reflected in alerts
at level B for hign Rint value (0.219) and low ratio of observed / Unique
reflections (38%).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0292P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method SHELXL
_refine_ls_extinction_coef 0.0051(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns 6864
_refine_ls_number_parameters 500
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.2315
_refine_ls_R_factor_gt 0.0661
_refine_ls_wR_factor_ref 0.1571
_refine_ls_wR_factor_gt 0.1043
_refine_ls_goodness_of_fit_ref 0.948
_refine_ls_restrained_S_all 0.948
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.72131(19) 0.8020(4) 0.03959(19) 0.0285(10) Uani 1 1 d . . .
C2 C 0.7300(2) 0.8893(5) -0.0068(2) 0.0275(12) Uani 1 1 d . . .
H2 H 0.7328 0.9902 -0.0038 0.033 Uiso 1 1 calc R . .
N3 N 0.73398(18) 0.8128(4) -0.05747(18) 0.0273(10) Uani 1 1 d . . .
C4 C 0.7279(2) 0.6706(5) -0.0436(2) 0.0349(14) Uani 1 1 d . . .
H4 H 0.7292 0.5924 -0.0713 0.042 Uiso 1 1 calc R . .
C5 C 0.7199(2) 0.6638(5) 0.0164(2) 0.0345(14) Uani 1 1 d . . .
H5 H 0.7142 0.5796 0.0390 0.041 Uiso 1 1 calc R . .
C1A C 0.7415(2) 0.8725(5) -0.1184(2) 0.0307(13) Uani 1 1 d . . .
H1A1 H 0.7125 0.9588 -0.1290 0.037 Uiso 1 1 calc R . .
H1A2 H 0.7240 0.8023 -0.1535 0.037 Uiso 1 1 calc R . .
N1' N 0.9147(2) 0.9273(4) -0.13158(19) 0.0331(11) Uani 1 1 d . . .
N2' N 0.9054(2) 1.0438(4) -0.0976(2) 0.0453(13) Uani 1 1 d . . .
N3' N 0.8434(2) 1.0333(4) -0.0892(2) 0.0411(12) Uani 1 1 d . . .
C4' C 0.8137(2) 0.9106(5) -0.1173(2) 0.0283(12) Uani 1 1 d . . .
C5' C 0.8588(3) 0.8441(5) -0.1442(2) 0.0322(13) Uani 1 1 d . . .
H5' H 0.8521 0.7566 -0.1672 0.039 Uiso 1 1 calc R . .
C6 C 0.7110(3) 0.8451(4) 0.1008(2) 0.0295(13) Uani 1 1 d . . .
C7 C 0.6439(3) 0.8602(4) 0.1056(2) 0.0298(13) Uani 1 1 d . . .
C8 C 0.6355(3) 0.9124(5) 0.1638(2) 0.0349(13) Uani 1 1 d . . .
H8 H 0.5900 0.9261 0.1678 0.042 Uiso 1 1 calc R . .
C9 C 0.6906(3) 0.9452(5) 0.2162(3) 0.0416(14) Uani 1 1 d . . .
C10 C 0.7567(3) 0.9251(5) 0.2089(2) 0.0389(14) Uani 1 1 d . . .
H10 H 0.7952 0.9450 0.2446 0.047 Uiso 1 1 calc R . .
C11 C 0.7685(3) 0.8770(5) 0.1515(3) 0.0338(13) Uani 1 1 d . . .
C12 C 0.5823(2) 0.8257(5) 0.0509(2) 0.0427(15) Uani 1 1 d . . .
H12A H 0.5964 0.8161 0.0107 0.064 Uiso 1 1 calc R . .
H12C H 0.5483 0.9025 0.0460 0.064 Uiso 1 1 calc R . .
H12D H 0.5618 0.7362 0.0600 0.064 Uiso 1 1 calc R . .
C13 C 0.6782(3) 1.0028(5) 0.2778(2) 0.0621(18) Uani 1 1 d . . .
H13A H 0.6600 0.9269 0.2999 0.093 Uiso 1 1 calc R . .
H13C H 0.6448 1.0810 0.2674 0.093 Uiso 1 1 calc R . .
H13D H 0.7218 1.0379 0.3061 0.093 Uiso 1 1 calc R . .
C14 C 0.8407(3) 0.8657(5) 0.1442(3) 0.0540(16) Uani 1 1 d . . .
H14A H 0.8489 0.9432 0.1165 0.081 Uiso 1 1 calc R . .
H14C H 0.8463 0.7740 0.1244 0.081 Uiso 1 1 calc R . .
H14D H 0.8739 0.8726 0.1869 0.081 Uiso 1 1 calc R . .
C6' C 0.9803(2) 0.9038(5) -0.1457(2) 0.0384(14) Uani 1 1 d . . .
H6'1 H 1.0092 0.9902 -0.1348 0.046 Uiso 1 1 calc R . .
H6'2 H 0.9726 0.8847 -0.1926 0.046 Uiso 1 1 calc R . .
C7' C 1.0171(2) 0.7784(5) -0.1069(2) 0.0330(13) Uani 1 1 d . . .
C8' C 1.0285(2) 0.6538(5) -0.1356(2) 0.0375(14) Uani 1 1 d . . .
H8' H 1.0166 0.6473 -0.1815 0.045 Uiso 1 1 calc R . .
C9' C 1.0573(2) 0.5366(5) -0.0983(3) 0.0402(14) Uani 1 1 d . . .
H9' H 1.0644 0.4497 -0.1183 0.048 Uiso 1 1 calc R . .
C10' C 1.0750(2) 0.5489(5) -0.0328(3) 0.0352(13) Uani 1 1 d . . .
C11' C 1.0673(2) 0.6751(5) -0.0018(2) 0.0399(14) Uani 1 1 d . . .
H11' H 1.0819 0.6825 0.0441 0.048 Uiso 1 1 calc R . .
C12' C 1.0380(2) 0.7892(5) -0.0395(2) 0.0400(14) Uani 1 1 d . . .
H12' H 1.0319 0.8766 -0.0194 0.048 Uiso 1 1 calc R . .
N4' N 1.1043(2) 0.4244(5) 0.0080(3) 0.0486(13) Uani 1 1 d . . .
O1' O 1.1220(2) 0.4403(4) 0.0665(2) 0.0684(13) Uani 1 1 d . . .
O2' O 1.1086(2) 0.3122(4) -0.0208(2) 0.0650(13) Uani 1 1 d . . .
B1B B 0.3802(3) 0.7218(5) 0.1172(3) 0.0254(14) Uani 1 1 d . . .
C11B C 0.3361(2) 0.6340(4) 0.1578(2) 0.0251(12) Uani 1 1 d . . .
C12B C 0.2718(2) 0.6805(5) 0.1637(2) 0.0292(12) Uani 1 1 d . . .
H12B H 0.2545 0.7691 0.1448 0.035 Uiso 1 1 calc R . .
C13B C 0.2324(2) 0.6043(5) 0.1957(2) 0.0322(13) Uani 1 1 d . . .
H13B H 0.1882 0.6387 0.1963 0.039 Uiso 1 1 calc R . .
C14B C 0.2567(3) 0.4780(5) 0.2270(2) 0.0331(13) Uani 1 1 d . . .
H14B H 0.2301 0.4255 0.2496 0.040 Uiso 1 1 calc R . .
C15B C 0.3208(3) 0.4310(5) 0.2241(2) 0.0317(13) Uani 1 1 d . . .
H15B H 0.3389 0.3454 0.2457 0.038 Uiso 1 1 calc R . .
C16B C 0.3588(2) 0.5062(4) 0.1905(2) 0.0263(12) Uani 1 1 d . . .
H16B H 0.4026 0.4697 0.1893 0.032 Uiso 1 1 calc R . .
C21B C 0.3382(2) 0.7359(4) 0.0397(2) 0.0245(12) Uani 1 1 d . . .
C22B C 0.2669(2) 0.7177(4) 0.0144(2) 0.0297(12) Uani 1 1 d . . .
H22B H 0.2403 0.6915 0.0431 0.036 Uiso 1 1 calc R . .
C23B C 0.2331(2) 0.7363(4) -0.0510(2) 0.0342(13) Uani 1 1 d . . .
H23B H 0.1845 0.7240 -0.0656 0.041 Uiso 1 1 calc R . .
C24B C 0.2700(3) 0.7726(5) -0.0948(2) 0.0383(14) Uani 1 1 d . . .
H24B H 0.2473 0.7859 -0.1393 0.046 Uiso 1 1 calc R . .
C25B C 0.3404(3) 0.7889(4) -0.0722(2) 0.0346(13) Uani 1 1 d . . .
H25B H 0.3667 0.8129 -0.1015 0.041 Uiso 1 1 calc R . .
C26B C 0.3731(2) 0.7705(4) -0.0070(2) 0.0274(12) Uani 1 1 d . . .
H26B H 0.4218 0.7819 0.0069 0.033 Uiso 1 1 calc R . .
C31B C 0.4531(2) 0.6382(4) 0.1241(2) 0.0247(12) Uani 1 1 d . . .
C32B C 0.4620(2) 0.5307(4) 0.0819(2) 0.0259(12) Uani 1 1 d . . .
H32B H 0.4248 0.5089 0.0454 0.031 Uiso 1 1 calc R . .
C33B C 0.5231(2) 0.4545(4) 0.0912(2) 0.0326(13) Uani 1 1 d . . .
H33B H 0.5262 0.3811 0.0616 0.039 Uiso 1 1 calc R . .
C34B C 0.5789(3) 0.4836(5) 0.1425(2) 0.0354(14) Uani 1 1 d . . .
H34B H 0.6211 0.4338 0.1477 0.042 Uiso 1 1 calc R . .
C35B C 0.5724(2) 0.5875(5) 0.1867(2) 0.0350(13) Uani 1 1 d . . .
H35B H 0.6096 0.6069 0.2235 0.042 Uiso 1 1 calc R . .
C36B C 0.5109(2) 0.6626(4) 0.1764(2) 0.0282(12) Uani 1 1 d . . .
H36B H 0.5079 0.7347 0.2066 0.034 Uiso 1 1 calc R . .
C41B C 0.3999(2) 0.8822(4) 0.1484(2) 0.0254(12) Uani 1 1 d . . .
C42B C 0.4234(2) 0.9925(4) 0.1157(2) 0.0304(13) Uani 1 1 d . . .
H42B H 0.4236 0.9778 0.0719 0.036 Uiso 1 1 calc R . .
C43B C 0.4461(2) 1.1219(5) 0.1443(3) 0.0376(14) Uani 1 1 d . . .
H43B H 0.4614 1.1933 0.1200 0.045 Uiso 1 1 calc R . .
C44B C 0.4470(2) 1.1483(5) 0.2076(3) 0.0349(14) Uani 1 1 d . . .
H44B H 0.4634 1.2366 0.2274 0.042 Uiso 1 1 calc R . .
C45B C 0.4236(2) 1.0442(5) 0.2418(2) 0.0319(13) Uani 1 1 d . . .
H45B H 0.4231 1.0607 0.2854 0.038 Uiso 1 1 calc R . .
C46B C 0.4005(2) 0.9144(5) 0.2122(2) 0.0278(12) Uani 1 1 d . . .
H46B H 0.3845 0.8444 0.2367 0.033 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.034(3) 0.022(3) 0.030(3) -0.005(2) 0.010(2) -0.0038(19)
C2 0.030(3) 0.022(3) 0.031(3) -0.003(3) 0.010(2) -0.003(2)
N3 0.027(2) 0.025(3) 0.026(3) -0.003(2) 0.000(2) 0.0061(19)
C4 0.041(4) 0.023(3) 0.038(4) -0.005(3) 0.006(3) 0.004(2)
C5 0.048(4) 0.018(3) 0.031(3) -0.002(3) -0.002(3) -0.005(2)
C1A 0.035(3) 0.031(3) 0.023(3) -0.001(2) 0.004(3) 0.006(2)
N1' 0.031(3) 0.034(3) 0.034(3) 0.003(2) 0.009(2) 0.007(2)
N2' 0.040(3) 0.036(3) 0.060(3) -0.014(2) 0.015(3) 0.006(2)
N3' 0.036(3) 0.036(3) 0.049(3) -0.010(2) 0.007(2) 0.004(2)
C4' 0.027(3) 0.031(3) 0.026(3) -0.002(2) 0.005(2) 0.004(3)
C5' 0.039(3) 0.027(3) 0.033(3) -0.005(3) 0.013(3) 0.002(3)
C6 0.033(3) 0.024(3) 0.030(3) 0.003(2) 0.004(3) -0.002(2)
C7 0.035(3) 0.022(3) 0.032(3) 0.005(2) 0.009(3) -0.003(2)
C8 0.039(3) 0.032(3) 0.041(4) 0.005(3) 0.021(3) -0.004(3)
C9 0.060(4) 0.032(3) 0.032(4) -0.004(3) 0.012(3) -0.007(3)
C10 0.052(4) 0.032(3) 0.027(3) 0.000(3) 0.002(3) -0.005(3)
C11 0.031(3) 0.030(3) 0.040(4) 0.001(3) 0.007(3) 0.001(2)
C12 0.036(3) 0.049(4) 0.041(4) 0.008(3) 0.007(3) -0.006(3)
C13 0.097(5) 0.057(4) 0.037(4) -0.003(3) 0.025(4) -0.001(3)
C14 0.043(4) 0.063(4) 0.050(4) -0.009(3) 0.003(3) -0.010(3)
C6' 0.033(3) 0.045(3) 0.039(4) 0.005(3) 0.012(3) 0.003(3)
C7' 0.024(3) 0.043(4) 0.030(3) 0.000(3) 0.004(3) 0.001(3)
C8' 0.038(3) 0.042(4) 0.032(3) -0.001(3) 0.007(3) 0.002(3)
C9' 0.033(3) 0.036(3) 0.048(4) -0.008(3) 0.005(3) -0.001(3)
C10' 0.028(3) 0.034(3) 0.041(4) 0.004(3) 0.006(3) 0.002(2)
C11' 0.037(3) 0.050(4) 0.030(3) 0.000(3) 0.004(3) 0.006(3)
C12' 0.044(4) 0.035(3) 0.040(4) -0.007(3) 0.008(3) 0.008(3)
N4' 0.037(3) 0.043(3) 0.061(4) 0.010(3) 0.004(3) 0.010(3)
O1' 0.093(4) 0.057(3) 0.042(3) 0.009(2) -0.005(3) 0.016(2)
O2' 0.066(3) 0.042(3) 0.084(3) 0.000(2) 0.016(2) 0.019(2)
B1B 0.034(4) 0.016(3) 0.026(3) 0.002(3) 0.008(3) 0.003(3)
C11B 0.029(3) 0.014(3) 0.031(3) -0.004(2) 0.006(2) -0.001(2)
C12B 0.039(3) 0.020(3) 0.029(3) -0.002(2) 0.009(3) -0.004(2)
C13B 0.029(3) 0.033(3) 0.037(3) -0.005(3) 0.015(3) -0.004(3)
C14B 0.037(3) 0.036(3) 0.031(3) -0.006(3) 0.018(3) -0.018(3)
C15B 0.049(4) 0.022(3) 0.026(3) 0.001(2) 0.013(3) -0.009(3)
C16B 0.028(3) 0.029(3) 0.023(3) 0.001(2) 0.008(2) -0.001(2)
C21B 0.026(3) 0.015(3) 0.035(3) 0.000(2) 0.012(3) 0.005(2)
C22B 0.031(3) 0.026(3) 0.033(3) 0.003(2) 0.011(3) 0.001(2)
C23B 0.032(3) 0.026(3) 0.042(4) 0.006(3) 0.006(3) -0.004(2)
C24B 0.050(4) 0.031(3) 0.027(3) 0.004(2) -0.003(3) 0.000(3)
C25B 0.046(4) 0.026(3) 0.034(3) 0.001(2) 0.013(3) 0.007(3)
C26B 0.026(3) 0.024(3) 0.032(3) -0.003(2) 0.007(3) 0.003(2)
C31B 0.034(3) 0.018(3) 0.024(3) 0.005(2) 0.011(2) 0.002(2)
C32B 0.028(3) 0.021(3) 0.027(3) 0.001(2) 0.005(2) -0.001(2)
C33B 0.039(3) 0.019(3) 0.040(4) -0.001(2) 0.013(3) 0.005(2)
C34B 0.034(3) 0.032(3) 0.041(4) 0.001(3) 0.011(3) 0.014(3)
C35B 0.028(3) 0.036(3) 0.036(3) -0.001(3) 0.001(3) 0.004(3)
C36B 0.032(3) 0.024(3) 0.031(3) -0.004(2) 0.012(3) 0.001(2)
C41B 0.022(3) 0.025(3) 0.027(3) 0.003(2) 0.003(2) 0.002(2)
C42B 0.032(3) 0.024(3) 0.036(3) 0.003(3) 0.010(3) -0.001(2)
C43B 0.043(4) 0.019(3) 0.052(4) 0.006(3) 0.013(3) -0.007(2)
C44B 0.031(3) 0.021(3) 0.047(4) -0.010(3) 0.002(3) 0.000(2)
C45B 0.032(3) 0.033(3) 0.030(3) -0.007(3) 0.006(3) 0.007(2)
C46B 0.028(3) 0.021(3) 0.032(3) 0.001(2) 0.005(3) 0.002(2)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C2 1.335(5) . ?
N1 C5 1.387(5) . ?
N1 C6 1.439(6) . ?
C2 N3 1.323(5) . ?
C2 H2 0.9500 . ?
N3 C4 1.381(5) . ?
N3 C1A 1.467(5) . ?
C4 C5 1.340(6) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C1A C4' 1.489(6) . ?
C1A H1A1 0.9900 . ?
C1A H1A2 0.9900 . ?
N1' C5' 1.337(5) . ?
N1' N2' 1.355(5) . ?
N1' C6' 1.448(5) . ?
N2' N3' 1.311(5) . ?
N3' C4' 1.361(5) . ?
C4' C5' 1.351(6) . ?
C5' H5' 0.9500 . ?
C6 C7 1.388(6) . ?
C6 C11 1.391(6) . ?
C7 C8 1.394(6) . ?
C7 C12 1.496(6) . ?
C8 C9 1.385(6) . ?
C8 H8 0.9500 . ?
C9 C10 1.392(7) . ?
C9 C13 1.508(6) . ?
C10 C11 1.390(6) . ?
C10 H10 0.9500 . ?
C11 C14 1.506(6) . ?
C12 H12A 0.9800 . ?
C12 H12C 0.9800 . ?
C12 H12D 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13C 0.9800 . ?
C13 H13D 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14C 0.9800 . ?
C14 H14D 0.9800 . ?
C6' C7' 1.516(6) . ?
C6' H6'1 0.9900 . ?
C6' H6'2 0.9900 . ?
C7' C8' 1.370(6) . ?
C7' C12' 1.395(6) . ?
C8' C9' 1.392(6) . ?
C8' H8' 0.9500 . ?
C9' C10' 1.359(6) . ?
C9' H9' 0.9500 . ?
C10' C11' 1.387(6) . ?
C10' N4' 1.485(6) . ?
C11' C12' 1.377(6) . ?
C11' H11' 0.9500 . ?
C12' H12' 0.9500 . ?
N4' O1' 1.216(5) . ?
N4' O2' 1.236(5) . ?
B1B C11B 1.623(7) . ?
B1B C31B 1.636(6) . ?
B1B C41B 1.653(6) . ?
B1B C21B 1.655(7) . ?
C11B C12B 1.403(6) . ?
C11B C16B 1.404(5) . ?
C12B C13B 1.379(6) . ?
C12B H12B 0.9500 . ?
C13B C14B 1.385(6) . ?
C13B H13B 0.9500 . ?
C14B C15B 1.380(6) . ?
C14B H14B 0.9500 . ?
C15B C16B 1.379(6) . ?
C15B H15B 0.9500 . ?
C16B H16B 0.9500 . ?
C21B C22B 1.402(6) . ?
C21B C26B 1.407(6) . ?
C22B C23B 1.395(6) . ?
C22B H22B 0.9500 . ?
C23B C24B 1.385(6) . ?
C23B H23B 0.9500 . ?
C24B C25B 1.377(6) . ?
C24B H24B 0.9500 . ?
C25B C26B 1.387(6) . ?
C25B H25B 0.9500 . ?
C26B H26B 0.9500 . ?
C31B C32B 1.398(6) . ?
C31B C36B 1.401(6) . ?
C32B C33B 1.389(6) . ?
C32B H32B 0.9500 . ?
C33B C34B 1.372(6) . ?
C33B H33B 0.9500 . ?
C34B C35B 1.390(6) . ?
C34B H34B 0.9500 . ?
C35B C36B 1.389(6) . ?
C35B H35B 0.9500 . ?
C36B H36B 0.9500 . ?
C41B C46B 1.399(6) . ?
C41B C42B 1.401(6) . ?
C42B C43B 1.383(6) . ?
C42B H42B 0.9500 . ?
C43B C44B 1.375(6) . ?
C43B H43B 0.9500 . ?
C44B C45B 1.378(6) . ?
C44B H44B 0.9500 . ?
C45B C46B 1.394(6) . ?
C45B H45B 0.9500 . ?
C46B H46B 0.9500 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 N1 C5 107.6(4) . . ?
C2 N1 C6 125.8(4) . . ?
C5 N1 C6 126.5(4) . . ?
N3 C2 N1 109.0(4) . . ?
N3 C2 H2 125.5 . . ?
N1 C2 H2 125.5 . . ?
C2 N3 C4 108.6(4) . . ?
C2 N3 C1A 124.6(4) . . ?
C4 N3 C1A 126.7(4) . . ?
C5 C4 N3 107.1(4) . . ?
C5 C4 H4 126.5 . . ?
N3 C4 H4 126.5 . . ?
C4 C5 N1 107.6(4) . . ?
C4 C5 H5 126.2 . . ?
N1 C5 H5 126.2 . . ?
N3 C1A C4' 114.2(4) . . ?
N3 C1A H1A1 108.7 . . ?
C4' C1A H1A1 108.7 . . ?
N3 C1A H1A2 108.7 . . ?
C4' C1A H1A2 108.7 . . ?
H1A1 C1A H1A2 107.6 . . ?
C5' N1' N2' 110.5(4) . . ?
C5' N1' C6' 129.3(4) . . ?
N2' N1' C6' 120.1(4) . . ?
N3' N2' N1' 106.7(4) . . ?
N2' N3' C4' 108.9(4) . . ?
C5' C4' N3' 108.3(4) . . ?
C5' C4' C1A 130.1(5) . . ?
N3' C4' C1A 121.4(4) . . ?
N1' C5' C4' 105.6(4) . . ?
N1' C5' H5' 127.2 . . ?
C4' C5' H5' 127.2 . . ?
C7 C6 C11 122.8(5) . . ?
C7 C6 N1 118.4(4) . . ?
C11 C6 N1 118.7(5) . . ?
C6 C7 C8 117.2(5) . . ?
C6 C7 C12 122.6(5) . . ?
C8 C7 C12 120.2(5) . . ?
C9 C8 C7 122.7(5) . . ?
C9 C8 H8 118.6 . . ?
C7 C8 H8 118.6 . . ?
C8 C9 C10 117.4(5) . . ?
C8 C9 C13 120.3(6) . . ?
C10 C9 C13 122.3(5) . . ?
C11 C10 C9 122.6(5) . . ?
C11 C10 H10 118.7 . . ?
C9 C10 H10 118.7 . . ?
C10 C11 C6 117.3(5) . . ?
C10 C11 C14 120.9(5) . . ?
C6 C11 C14 121.8(5) . . ?
C7 C12 H12A 109.5 . . ?
C7 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
C7 C12 H12D 109.5 . . ?
H12A C12 H12D 109.5 . . ?
H12C C12 H12D 109.5 . . ?
C9 C13 H13A 109.5 . . ?
C9 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
C9 C13 H13D 109.5 . . ?
H13A C13 H13D 109.5 . . ?
H13C C13 H13D 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
C11 C14 H14D 109.5 . . ?
H14A C14 H14D 109.5 . . ?
H14C C14 H14D 109.5 . . ?
N1' C6' C7' 110.0(4) . . ?
N1' C6' H6'1 109.7 . . ?
C7' C6' H6'1 109.7 . . ?
N1' C6' H6'2 109.7 . . ?
C7' C6' H6'2 109.7 . . ?
H6'1 C6' H6'2 108.2 . . ?
C8' C7' C12' 119.1(5) . . ?
C8' C7' C6' 122.2(5) . . ?
C12' C7' C6' 118.7(5) . . ?
C7' C8' C9' 120.8(5) . . ?
C7' C8' H8' 119.6 . . ?
C9' C8' H8' 119.6 . . ?
C10' C9' C8' 118.7(5) . . ?
C10' C9' H9' 120.7 . . ?
C8' C9' H9' 120.7 . . ?
C9' C10' C11' 122.4(5) . . ?
C9' C10' N4' 119.6(5) . . ?
C11' C10' N4' 117.9(5) . . ?
C12' C11' C10' 117.9(5) . . ?
C12' C11' H11' 121.0 . . ?
C10' C11' H11' 121.0 . . ?
C11' C12' C7' 121.0(5) . . ?
C11' C12' H12' 119.5 . . ?
C7' C12' H12' 119.5 . . ?
O1' N4' O2' 125.4(5) . . ?
O1' N4' C10' 118.0(5) . . ?
O2' N4' C10' 116.5(5) . . ?
C11B B1B C31B 108.3(4) . . ?
C11B B1B C41B 110.7(4) . . ?
C31B B1B C41B 106.8(4) . . ?
C11B B1B C21B 111.9(4) . . ?
C31B B1B C21B 109.5(4) . . ?
C41B B1B C21B 109.6(3) . . ?
C12B C11B C16B 114.0(4) . . ?
C12B C11B B1B 122.7(4) . . ?
C16B C11B B1B 123.4(4) . . ?
C13B C12B C11B 123.4(4) . . ?
C13B C12B H12B 118.3 . . ?
C11B C12B H12B 118.3 . . ?
C12B C13B C14B 120.7(5) . . ?
C12B C13B H13B 119.6 . . ?
C14B C13B H13B 119.6 . . ?
C15B C14B C13B 117.7(4) . . ?
C15B C14B H14B 121.2 . . ?
C13B C14B H14B 121.2 . . ?
C16B C15B C14B 121.1(4) . . ?
C16B C15B H15B 119.5 . . ?
C14B C15B H15B 119.5 . . ?
C15B C16B C11B 123.1(5) . . ?
C15B C16B H16B 118.4 . . ?
C11B C16B H16B 118.4 . . ?
C22B C21B C26B 114.0(4) . . ?
C22B C21B B1B 125.0(4) . . ?
C26B C21B B1B 121.0(4) . . ?
C23B C22B C21B 123.1(5) . . ?
C23B C22B H22B 118.4 . . ?
C21B C22B H22B 118.4 . . ?
C24B C23B C22B 120.4(5) . . ?
C24B C23B H23B 119.8 . . ?
C22B C23B H23B 119.8 . . ?
C25B C24B C23B 118.5(5) . . ?
C25B C24B H24B 120.8 . . ?
C23B C24B H24B 120.8 . . ?
C24B C25B C26B 120.4(5) . . ?
C24B C25B H25B 119.8 . . ?
C26B C25B H25B 119.8 . . ?
C25B C26B C21B 123.6(4) . . ?
C25B C26B H26B 118.2 . . ?
C21B C26B H26B 118.2 . . ?
C32B C31B C36B 114.4(4) . . ?
C32B C31B B1B 123.7(4) . . ?
C36B C31B B1B 121.7(4) . . ?
C33B C32B C31B 122.7(4) . . ?
C33B C32B H32B 118.6 . . ?
C31B C32B H32B 118.6 . . ?
C34B C33B C32B 121.0(5) . . ?
C34B C33B H33B 119.5 . . ?
C32B C33B H33B 119.5 . . ?
C33B C34B C35B 118.6(5) . . ?
C33B C34B H34B 120.7 . . ?
C35B C34B H34B 120.7 . . ?
C36B C35B C34B 119.4(5) . . ?
C36B C35B H35B 120.3 . . ?
C34B C35B H35B 120.3 . . ?
C35B C36B C31B 123.8(4) . . ?
C35B C36B H36B 118.1 . . ?
C31B C36B H36B 118.1 . . ?
C46B C41B C42B 114.4(4) . . ?
C46B C41B B1B 122.1(4) . . ?
C42B C41B B1B 123.3(4) . . ?
C43B C42B C41B 123.0(5) . . ?
C43B C42B H42B 118.5 . . ?
C41B C42B H42B 118.5 . . ?
C44B C43B C42B 120.8(5) . . ?
C44B C43B H43B 119.6 . . ?
C42B C43B H43B 119.6 . . ?
C43B C44B C45B 118.7(4) . . ?
C43B C44B H44B 120.7 . . ?
C45B C44B H44B 120.7 . . ?
C44B C45B C46B 119.9(5) . . ?
C44B C45B H45B 120.1 . . ?
C46B C45B H45B 120.1 . . ?
C45B C46B C41B 123.3(4) . . ?
C45B C46B H46B 118.4 . . ?
C41B C46B H46B 118.4 . . ?
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max 0.236
_refine_diff_density_min -0.304
_refine_diff_density_rms 0.059
_database_code_depnum_ccdc_archive 'CCDC 934041'
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_inp1bar4
#TrackingRef 'Marina1_Deposition_15Jun11.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C32 H38 Cl Ir N5, C24 H20 B, 2(C H2 Cl2)'
_chemical_formula_sum 'C58 H62 B Cl5 Ir N5'
_chemical_formula_weight 1209.39
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Triclinic
_symmetry_space_group_name_H-M P-1
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 13.4189(7)
_cell_length_b 13.6633(7)
_cell_length_c 14.7206(8)
_cell_angle_alpha 89.731(2)
_cell_angle_beta 83.712(2)
_cell_angle_gamma 85.488(2)
_cell_volume 2674.4(2)
_cell_formula_units_Z 2
_cell_measurement_temperature 155(2)
_cell_measurement_reflns_used 9855
_cell_measurement_theta_min 2.784
_cell_measurement_theta_max 30.514
_exptl_crystal_description Blocks
_exptl_crystal_colour Yellow
_exptl_crystal_size_max 0.24
_exptl_crystal_size_mid 0.17
_exptl_crystal_size_min 0.14
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.502
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1224
_exptl_absorpt_coefficient_mu 2.789
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.5565
_exptl_absorpt_correction_T_max 0.6978
_exptl_absorpt_process_details 'SADABS (Bruker, 2001)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 155(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker kappa APEXII CCD Diffractometer'
_diffrn_measurement_method '\f scans, and \w scans with \k offsets'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 36887
_diffrn_reflns_av_R_equivalents 0.0227
_diffrn_reflns_av_sigmaI/netI 0.0199
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_theta_min 3.47
_diffrn_reflns_theta_max 24.99
_reflns_number_total 9359
_reflns_number_gt 8757
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2007)'
_computing_cell_refinement 'APEX2 (Bruker, 2007)'
_computing_data_reduction 'APEX2 (Bruker, 2007)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0208P)^2^+3.3683P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 9359
_refine_ls_number_parameters 639
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0226
_refine_ls_R_factor_gt 0.0191
_refine_ls_wR_factor_ref 0.0499
_refine_ls_wR_factor_gt 0.0472
_refine_ls_goodness_of_fit_ref 1.068
_refine_ls_restrained_S_all 1.068
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir1 Ir 0.779242(6) 0.763913(7) 0.733921(6) 0.01608(4) Uani 1 1 d . . .
Cl2 Cl 0.79639(5) 0.72172(5) 0.88916(4) 0.02487(13) Uani 1 1 d . . .
Cl1D Cl 0.98770(8) 0.44663(9) 0.84299(7) 0.0694(3) Uani 1 1 d . . .
Cl2D Cl 0.86503(9) 0.40218(11) 1.00920(8) 0.0828(4) Uani 1 1 d . . .
Cl1E Cl 0.97150(7) 0.86819(8) 0.11907(7) 0.0595(2) Uani 1 1 d . . .
Cl2E Cl 0.81161(8) 0.74315(7) 0.17544(8) 0.0653(3) Uani 1 1 d . . .
B1C B 0.2869(2) 0.7563(2) 0.5387(2) 0.0205(6) Uani 1 1 d . . .
C11C C 0.19345(19) 0.76249(19) 0.47417(17) 0.0235(6) Uani 1 1 d . . .
C16C C 0.1116(2) 0.8328(2) 0.4824(2) 0.0308(6) Uani 1 1 d . . .
H16C H 0.1082 0.8821 0.5282 0.037 Uiso 1 1 calc R . .
C13C C 0.1149(2) 0.6903(3) 0.3498(2) 0.0453(8) Uani 1 1 d . . .
H13C H 0.1168 0.6402 0.3050 0.054 Uiso 1 1 calc R . .
C12C C 0.1912(2) 0.6916(2) 0.40578(19) 0.0329(7) Uani 1 1 d . . .
H12C H 0.2450 0.6418 0.3975 0.039 Uiso 1 1 calc R . .
C15C C 0.0345(2) 0.8332(3) 0.4257(2) 0.0442(8) Uani 1 1 d . . .
H15C H -0.0195 0.8828 0.4330 0.053 Uiso 1 1 calc R . .
C14C C 0.0363(3) 0.7618(3) 0.3592(2) 0.0495(9) Uani 1 1 d . . .
H14C H -0.0159 0.7620 0.3205 0.059 Uiso 1 1 calc R . .
C21C C 0.29649(18) 0.86363(18) 0.58615(17) 0.0204(5) Uani 1 1 d . . .
C26C C 0.37679(19) 0.92244(19) 0.56452(17) 0.0234(5) Uani 1 1 d . . .
H26C H 0.4319 0.8975 0.5228 0.028 Uiso 1 1 calc R . .
C22C C 0.2207(2) 0.9050(2) 0.65168(18) 0.0263(6) Uani 1 1 d . . .
H22C H 0.1662 0.8671 0.6719 0.032 Uiso 1 1 calc R . .
C23C C 0.2217(2) 0.9983(2) 0.68817(19) 0.0290(6) Uani 1 1 d . . .
H23C H 0.1676 1.0236 0.7307 0.035 Uiso 1 1 calc R . .
C25C C 0.3793(2) 1.0159(2) 0.60155(19) 0.0294(6) Uani 1 1 d . . .
H25C H 0.4352 1.0530 0.5844 0.035 Uiso 1 1 calc R . .
C24C C 0.3014(2) 1.0547(2) 0.66279(19) 0.0293(6) Uani 1 1 d . . .
H24C H 0.3023 1.1189 0.6871 0.035 Uiso 1 1 calc R . .
C34C C 0.5761(2) 0.6844(2) 0.35960(19) 0.0277(6) Uani 1 1 d . . .
H34C H 0.6382 0.6716 0.3224 0.033 Uiso 1 1 calc R . .
C32C C 0.41975(19) 0.78133(18) 0.39575(17) 0.0213(5) Uani 1 1 d . . .
H32C H 0.3749 0.8348 0.3807 0.026 Uiso 1 1 calc R . .
C31C C 0.39137(18) 0.72464(18) 0.47284(17) 0.0193(5) Uani 1 1 d . . .
C36C C 0.45964(19) 0.64506(18) 0.48815(18) 0.0224(5) Uani 1 1 d . . .
H36C H 0.4434 0.6028 0.5381 0.027 Uiso 1 1 calc R . .
C33C C 0.5095(2) 0.76317(19) 0.34083(18) 0.0245(6) Uani 1 1 d . . .
H33C H 0.5258 0.8046 0.2902 0.029 Uiso 1 1 calc R . .
C35C C 0.5503(2) 0.6251(2) 0.43334(19) 0.0271(6) Uani 1 1 d . . .
H35C H 0.5946 0.5705 0.4467 0.032 Uiso 1 1 calc R . .
C41C C 0.26689(18) 0.67201(18) 0.61851(17) 0.0208(5) Uani 1 1 d . . .
C42C C 0.29561(18) 0.6805(2) 0.70666(18) 0.0246(6) Uani 1 1 d . . .
H42C H 0.3255 0.7382 0.7218 0.029 Uiso 1 1 calc R . .
C46C C 0.2230(2) 0.5850(2) 0.60231(19) 0.0282(6) Uani 1 1 d . . .
H46C H 0.2018 0.5751 0.5438 0.034 Uiso 1 1 calc R . .
C43C C 0.2824(2) 0.6085(2) 0.7729(2) 0.0300(6) Uani 1 1 d . . .
H43C H 0.3033 0.6176 0.8317 0.036 Uiso 1 1 calc R . .
C45C C 0.2090(2) 0.5125(2) 0.6678(2) 0.0318(7) Uani 1 1 d . . .
H45C H 0.1786 0.4548 0.6536 0.038 Uiso 1 1 calc R . .
C44C C 0.2392(2) 0.5239(2) 0.7535(2) 0.0317(7) Uani 1 1 d . . .
H44C H 0.2303 0.4742 0.7984 0.038 Uiso 1 1 calc R . .
C1D C 0.8837(3) 0.4840(3) 0.9196(3) 0.0623(11) Uani 1 1 d . . .
H1D1 H 0.8932 0.5494 0.9445 0.075 Uiso 1 1 calc R . .
H1D2 H 0.8230 0.4904 0.8867 0.075 Uiso 1 1 calc R . .
C9A C 0.9319(2) 0.5895(2) 0.6188(2) 0.0335(7) Uani 1 1 d . . .
H9A1 H 0.9825 0.5822 0.5655 0.050 Uiso 1 1 calc R . .
H9A2 H 0.8717 0.5580 0.6062 0.050 Uiso 1 1 calc R . .
H9A3 H 0.9591 0.5584 0.6719 0.050 Uiso 1 1 calc R . .
C3A C 0.83566(19) 0.75805(19) 0.59002(17) 0.0229(5) Uani 1 1 d . . .
C1A C 0.90102(18) 0.85581(18) 0.69463(18) 0.0221(5) Uani 1 1 d . . .
C6A C 0.9327(2) 0.9419(2) 0.7425(2) 0.0301(6) Uani 1 1 d . . .
H6A1 H 1.0003 0.9563 0.7163 0.045 Uiso 1 1 calc R . .
H6A2 H 0.9334 0.9270 0.8077 0.045 Uiso 1 1 calc R . .
H6A3 H 0.8854 0.9990 0.7352 0.045 Uiso 1 1 calc R . .
C2A C 0.83591(19) 0.85620(19) 0.62231(18) 0.0236(6) Uani 1 1 d . . .
C4A C 0.90490(18) 0.69587(19) 0.63816(18) 0.0222(5) Uani 1 1 d . . .
C10A C 1.0200(2) 0.7219(2) 0.7646(2) 0.0300(6) Uani 1 1 d . . .
H10A H 1.0094 0.6544 0.7839 0.045 Uiso 1 1 calc R . .
H10B H 1.0115 0.7651 0.8184 0.045 Uiso 1 1 calc R . .
H10C H 1.0882 0.7244 0.7336 0.045 Uiso 1 1 calc R . .
C5A C 0.94534(18) 0.75518(19) 0.70084(18) 0.0227(5) Uani 1 1 d . . .
C7A C 0.7828(2) 0.9437(2) 0.5818(2) 0.0332(7) Uani 1 1 d . . .
H7A1 H 0.7952 1.0032 0.6144 0.050 Uiso 1 1 calc R . .
H7A2 H 0.7104 0.9360 0.5874 0.050 Uiso 1 1 calc R . .
H7A3 H 0.8081 0.9492 0.5171 0.050 Uiso 1 1 calc R . .
C8A C 0.7858(2) 0.7261(2) 0.50995(19) 0.0340(7) Uani 1 1 d . . .
H8A1 H 0.7347 0.7773 0.4956 0.051 Uiso 1 1 calc R . .
H8A2 H 0.7539 0.6651 0.5250 0.051 Uiso 1 1 calc R . .
H8A3 H 0.8363 0.7149 0.4569 0.051 Uiso 1 1 calc R . .
C1E C 0.8950(3) 0.7813(3) 0.0834(2) 0.0462(8) Uani 1 1 d . . .
H1E1 H 0.9376 0.7237 0.0570 0.055 Uiso 1 1 calc R . .
H1E2 H 0.8560 0.8100 0.0351 0.055 Uiso 1 1 calc R . .
N2B N 0.70415(15) 0.55795(15) 0.75990(14) 0.0202(4) Uani 1 1 d . . .
N3B N 0.62539(15) 0.51019(15) 0.74223(14) 0.0203(4) Uani 1 1 d . . .
N1B N 0.68425(15) 0.64921(15) 0.73277(13) 0.0185(4) Uani 1 1 d . . .
N5B N 0.61638(16) 0.91688(17) 0.83922(16) 0.0277(5) Uani 1 1 d . . .
N4B N 0.56139(15) 0.83130(15) 0.73689(15) 0.0211(5) Uani 1 1 d . . .
C3B C 0.55633(19) 0.75703(18) 0.66612(17) 0.0213(5) Uani 1 1 d . . .
H3B1 H 0.5979 0.7743 0.6094 0.026 Uiso 1 1 calc R . .
H3B2 H 0.4860 0.7550 0.6522 0.026 Uiso 1 1 calc R . .
C2B C 0.59392(18) 0.65909(18) 0.69911(16) 0.0183(5) Uani 1 1 d . . .
C6B C 0.64702(18) 0.84645(18) 0.77476(17) 0.0200(5) Uani 1 1 d . . .
C1B C 0.55547(19) 0.56956(19) 0.70527(17) 0.0219(5) Uani 1 1 d . . .
H1B H 0.4931 0.5527 0.6874 0.026 Uiso 1 1 calc R . .
C4B C 0.4795(2) 0.8892(2) 0.7765(2) 0.0328(7) Uani 1 1 d . . .
H4B H 0.4123 0.8908 0.7616 0.039 Uiso 1 1 calc R . .
C5B C 0.5140(2) 0.9427(2) 0.8402(2) 0.0392(8) Uani 1 1 d . . .
H5B H 0.4754 0.9900 0.8793 0.047 Uiso 1 1 calc R . .
C14B C 0.67408(19) 0.96678(19) 0.90003(19) 0.0246(6) Uani 1 1 d . . .
C19B C 0.7153(2) 1.05327(19) 0.87027(18) 0.0255(6) Uani 1 1 d . . .
C18B C 0.7672(2) 1.10219(19) 0.93060(18) 0.0260(6) Uani 1 1 d . . .
H18B H 0.7988 1.1595 0.9104 0.031 Uiso 1 1 calc R . .
C17B C 0.7743(2) 1.0700(2) 1.01897(19) 0.0265(6) Uani 1 1 d . . .
C8B C 0.5690(2) 0.39009(18) 0.86012(19) 0.0251(6) Uani 1 1 d . . .
C7B C 0.6212(2) 0.40573(18) 0.76612(19) 0.0258(6) Uani 1 1 d . . .
H7B1 H 0.6906 0.3743 0.7625 0.031 Uiso 1 1 calc R . .
H7B2 H 0.5855 0.3731 0.7208 0.031 Uiso 1 1 calc R . .
C16B C 0.7255(2) 0.98744(19) 1.04808(19) 0.0265(6) Uani 1 1 d . . .
H16B H 0.7276 0.9662 1.1094 0.032 Uiso 1 1 calc R . .
C15B C 0.67377(19) 0.93491(19) 0.99027(19) 0.0253(6) Uani 1 1 d . . .
C20B C 0.6156(2) 0.8510(2) 1.0267(2) 0.0369(7) Uani 1 1 d . . .
H20A H 0.6226 0.8425 1.0919 0.055 Uiso 1 1 calc R . .
H20B H 0.6419 0.7907 0.9937 0.055 Uiso 1 1 calc R . .
H20C H 0.5444 0.8649 1.0183 0.055 Uiso 1 1 calc R . .
C9B C 0.6218(3) 0.3454(2) 0.9267(2) 0.0392(7) Uani 1 1 d . . .
H9B H 0.6914 0.3259 0.9133 0.047 Uiso 1 1 calc R . .
C22B C 0.6983(3) 1.0994(2) 0.7796(2) 0.0373(7) Uani 1 1 d . . .
H22A H 0.6407 1.1485 0.7879 0.056 Uiso 1 1 calc R . .
H22B H 0.6847 1.0486 0.7369 0.056 Uiso 1 1 calc R . .
H22D H 0.7585 1.1311 0.7550 0.056 Uiso 1 1 calc R . .
C10B C 0.5732(4) 0.3288(3) 1.0130(2) 0.0578(11) Uani 1 1 d . . .
H10D H 0.6094 0.2968 1.0581 0.069 Uiso 1 1 calc R . .
C12B C 0.4205(3) 0.4020(2) 0.9680(3) 0.0535(10) Uani 1 1 d . . .
H12B H 0.3511 0.4218 0.9821 0.064 Uiso 1 1 calc R . .
C13B C 0.4677(2) 0.4174(2) 0.8811(2) 0.0385(7) Uani 1 1 d . . .
H13B H 0.4301 0.4469 0.8357 0.046 Uiso 1 1 calc R . .
C21B C 0.8304(3) 1.1253(2) 1.0834(2) 0.0393(7) Uani 1 1 d . . .
H21A H 0.8933 1.0871 1.0931 0.059 Uiso 1 1 calc R . .
H21B H 0.7887 1.1356 1.1420 0.059 Uiso 1 1 calc R . .
H21C H 0.8457 1.1890 1.0567 0.059 Uiso 1 1 calc R . .
C11B C 0.4738(4) 0.3584(3) 1.0334(2) 0.0590(12) Uani 1 1 d . . .
H11B H 0.4415 0.3487 1.0931 0.071 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ir1 0.01290(5) 0.01538(6) 0.02005(6) -0.00203(4) -0.00153(4) -0.00192(3)
Cl2 0.0234(3) 0.0295(3) 0.0216(3) -0.0015(3) -0.0041(2) 0.0008(3)
Cl1D 0.0683(7) 0.0807(7) 0.0557(6) 0.0134(5) 0.0023(5) 0.0020(5)
Cl2D 0.0590(6) 0.1247(11) 0.0634(7) 0.0297(7) 0.0020(5) -0.0128(7)
Cl1E 0.0443(5) 0.0736(7) 0.0616(6) -0.0153(5) -0.0047(4) -0.0125(4)
Cl2E 0.0527(6) 0.0485(5) 0.0904(8) 0.0003(5) 0.0079(5) -0.0002(4)
B1C 0.0186(14) 0.0210(15) 0.0216(15) -0.0003(11) -0.0001(11) -0.0028(11)
C11C 0.0194(13) 0.0278(14) 0.0234(13) 0.0062(11) 0.0002(10) -0.0072(11)
C16C 0.0233(14) 0.0295(15) 0.0393(17) 0.0092(12) -0.0026(12) -0.0031(12)
C13C 0.0397(19) 0.068(2) 0.0322(17) -0.0024(16) -0.0083(14) -0.0216(17)
C12C 0.0264(15) 0.0438(18) 0.0296(15) -0.0018(13) -0.0038(12) -0.0084(13)
C15C 0.0233(15) 0.054(2) 0.056(2) 0.0232(17) -0.0073(14) -0.0048(14)
C14C 0.0327(18) 0.080(3) 0.0410(19) 0.0170(18) -0.0159(15) -0.0211(18)
C21C 0.0193(12) 0.0211(13) 0.0209(13) 0.0023(10) -0.0026(10) -0.0012(10)
C26C 0.0219(13) 0.0262(14) 0.0218(13) -0.0024(11) 0.0003(10) -0.0040(11)
C22C 0.0258(14) 0.0243(14) 0.0277(14) 0.0001(11) 0.0050(11) -0.0063(11)
C23C 0.0303(15) 0.0258(15) 0.0286(15) -0.0063(11) 0.0048(12) 0.0009(12)
C25C 0.0292(15) 0.0292(15) 0.0305(15) -0.0018(12) -0.0002(12) -0.0117(12)
C24C 0.0384(16) 0.0206(14) 0.0289(15) -0.0050(11) -0.0028(12) -0.0041(12)
C34C 0.0166(13) 0.0316(15) 0.0341(15) -0.0102(12) 0.0040(11) -0.0057(11)
C32C 0.0233(13) 0.0193(13) 0.0220(13) -0.0017(10) -0.0045(10) -0.0037(10)
C31C 0.0187(12) 0.0188(13) 0.0214(13) -0.0033(10) -0.0030(10) -0.0052(10)
C36C 0.0228(13) 0.0196(13) 0.0254(13) -0.0011(10) -0.0041(11) -0.0047(10)
C33C 0.0279(14) 0.0245(14) 0.0217(13) -0.0043(10) 0.0011(11) -0.0105(11)
C35C 0.0207(13) 0.0219(14) 0.0387(16) -0.0067(12) -0.0051(12) 0.0005(11)
C41C 0.0149(12) 0.0191(13) 0.0270(14) -0.0009(10) 0.0028(10) 0.0007(10)
C42C 0.0151(12) 0.0284(14) 0.0302(14) 0.0026(11) -0.0015(10) -0.0030(10)
C46C 0.0307(15) 0.0243(14) 0.0285(15) -0.0036(11) 0.0033(12) -0.0038(11)
C43C 0.0196(13) 0.0400(17) 0.0302(15) 0.0087(12) -0.0025(11) -0.0015(12)
C45C 0.0318(15) 0.0191(14) 0.0427(17) 0.0012(12) 0.0064(13) -0.0051(11)
C44C 0.0245(14) 0.0295(15) 0.0381(17) 0.0137(12) 0.0059(12) 0.0028(12)
C1D 0.053(2) 0.053(2) 0.078(3) 0.016(2) -0.006(2) 0.0098(19)
C9A 0.0291(15) 0.0266(15) 0.0431(17) -0.0076(13) 0.0023(13) -0.0002(12)
C3A 0.0217(13) 0.0275(14) 0.0187(13) -0.0016(10) 0.0041(10) -0.0064(11)
C1A 0.0181(12) 0.0175(13) 0.0308(14) -0.0041(10) 0.0007(10) -0.0059(10)
C6A 0.0228(14) 0.0234(14) 0.0450(17) -0.0041(12) -0.0045(12) -0.0061(11)
C2A 0.0216(13) 0.0245(14) 0.0241(13) 0.0026(11) 0.0029(10) -0.0067(11)
C4A 0.0167(12) 0.0227(13) 0.0255(13) -0.0037(10) 0.0073(10) -0.0027(10)
C10A 0.0164(13) 0.0307(15) 0.0429(17) -0.0007(13) -0.0033(12) -0.0013(11)
C5A 0.0133(12) 0.0249(14) 0.0288(14) -0.0012(11) 0.0047(10) -0.0049(10)
C7A 0.0376(16) 0.0287(15) 0.0332(16) 0.0081(12) -0.0036(13) -0.0029(13)
C8A 0.0352(16) 0.0431(18) 0.0244(15) -0.0041(13) -0.0007(12) -0.0107(13)
C1E 0.049(2) 0.047(2) 0.0420(19) -0.0153(15) -0.0096(16) 0.0070(16)
N2B 0.0203(11) 0.0176(11) 0.0225(11) -0.0018(8) -0.0004(9) -0.0026(8)
N3B 0.0212(11) 0.0167(11) 0.0236(11) -0.0024(8) -0.0017(9) -0.0057(9)
N1B 0.0179(10) 0.0195(11) 0.0176(10) -0.0038(8) -0.0002(8) -0.0018(8)
N5B 0.0179(11) 0.0272(12) 0.0382(13) -0.0141(10) -0.0067(10) 0.0038(9)
N4B 0.0153(10) 0.0205(11) 0.0280(12) -0.0037(9) -0.0055(9) 0.0010(8)
C3B 0.0201(13) 0.0198(13) 0.0250(13) -0.0021(10) -0.0058(10) -0.0037(10)
C2B 0.0164(12) 0.0212(13) 0.0173(12) -0.0026(10) -0.0017(9) -0.0022(10)
C6B 0.0198(13) 0.0163(12) 0.0245(13) -0.0019(10) -0.0044(10) -0.0020(10)
C1B 0.0195(13) 0.0236(13) 0.0238(13) -0.0019(10) -0.0044(10) -0.0064(10)
C4B 0.0174(13) 0.0339(16) 0.0467(18) -0.0115(13) -0.0066(12) 0.0052(12)
C5B 0.0192(14) 0.0420(18) 0.056(2) -0.0257(15) -0.0075(13) 0.0091(13)
C14B 0.0173(13) 0.0232(14) 0.0332(15) -0.0136(11) -0.0050(11) 0.0042(10)
C19B 0.0250(14) 0.0232(14) 0.0277(14) -0.0055(11) -0.0059(11) 0.0055(11)
C18B 0.0286(14) 0.0196(13) 0.0303(15) -0.0023(11) -0.0045(11) -0.0027(11)
C17B 0.0270(14) 0.0238(14) 0.0290(15) -0.0069(11) -0.0045(11) -0.0021(11)
C8B 0.0314(15) 0.0125(12) 0.0319(15) -0.0024(10) -0.0018(12) -0.0067(11)
C7B 0.0298(14) 0.0164(13) 0.0315(15) -0.0027(11) -0.0018(12) -0.0046(11)
C16B 0.0289(14) 0.0246(14) 0.0248(14) -0.0045(11) -0.0002(11) 0.0009(11)
C15B 0.0192(13) 0.0195(13) 0.0354(15) -0.0076(11) 0.0032(11) 0.0021(10)
C20B 0.0333(16) 0.0264(15) 0.0480(19) -0.0115(13) 0.0121(14) -0.0070(13)
C9B 0.0477(19) 0.0324(17) 0.0407(18) 0.0014(14) -0.0134(15) -0.0108(14)
C22B 0.0476(19) 0.0327(17) 0.0329(16) -0.0024(13) -0.0158(14) 0.0054(14)
C10B 0.094(3) 0.051(2) 0.0342(19) 0.0067(16) -0.019(2) -0.028(2)
C12B 0.056(2) 0.0299(18) 0.069(3) -0.0081(17) 0.029(2) -0.0134(16)
C13B 0.0335(16) 0.0252(15) 0.054(2) 0.0058(14) 0.0061(14) -0.0037(13)
C21B 0.052(2) 0.0368(18) 0.0327(16) -0.0037(13) -0.0135(14) -0.0147(15)
C11B 0.101(3) 0.039(2) 0.036(2) -0.0110(16) 0.018(2) -0.038(2)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ir1 C6B 2.059(2) . ?
Ir1 N1B 2.098(2) . ?
Ir1 C1A 2.166(2) . ?
Ir1 C3A 2.170(2) . ?
Ir1 C2A 2.174(2) . ?
Ir1 C4A 2.222(2) . ?
Ir1 C5A 2.223(2) . ?
Ir1 Cl2 2.3852(6) . ?
Cl1D C1D 1.740(4) . ?
Cl2D C1D 1.735(4) . ?
Cl1E C1E 1.748(4) . ?
Cl2E C1E 1.765(4) . ?
B1C C31C 1.645(4) . ?
B1C C21C 1.647(4) . ?
B1C C11C 1.651(4) . ?
B1C C41C 1.656(4) . ?
C11C C16C 1.396(4) . ?
C11C C12C 1.405(4) . ?
C16C C15C 1.398(4) . ?
C16C H16C 0.9500 . ?
C13C C14C 1.376(5) . ?
C13C C12C 1.384(4) . ?
C13C H13C 0.9500 . ?
C12C H12C 0.9500 . ?
C15C C14C 1.383(5) . ?
C15C H15C 0.9500 . ?
C14C H14C 0.9500 . ?
C21C C26C 1.403(4) . ?
C21C C22C 1.408(4) . ?
C26C C25C 1.395(4) . ?
C26C H26C 0.9500 . ?
C22C C23C 1.388(4) . ?
C22C H22C 0.9500 . ?
C23C C24C 1.384(4) . ?
C23C H23C 0.9500 . ?
C25C C24C 1.378(4) . ?
C25C H25C 0.9500 . ?
C24C H24C 0.9500 . ?
C34C C35C 1.381(4) . ?
C34C C33C 1.390(4) . ?
C34C H34C 0.9500 . ?
C32C C33C 1.381(4) . ?
C32C C31C 1.406(3) . ?
C32C H32C 0.9500 . ?
C31C C36C 1.399(4) . ?
C36C C35C 1.393(4) . ?
C36C H36C 0.9500 . ?
C33C H33C 0.9500 . ?
C35C H35C 0.9500 . ?
C41C C46C 1.401(4) . ?
C41C C42C 1.401(4) . ?
C42C C43C 1.389(4) . ?
C42C H42C 0.9500 . ?
C46C C45C 1.388(4) . ?
C46C H46C 0.9500 . ?
C43C C44C 1.378(4) . ?
C43C H43C 0.9500 . ?
C45C C44C 1.379(4) . ?
C45C H45C 0.9500 . ?
C44C H44C 0.9500 . ?
C1D H1D1 0.9900 . ?
C1D H1D2 0.9900 . ?
C9A C4A 1.491(4) . ?
C9A H9A1 0.9800 . ?
C9A H9A2 0.9800 . ?
C9A H9A3 0.9800 . ?
C3A C2A 1.425(4) . ?
C3A C4A 1.450(4) . ?
C3A C8A 1.500(4) . ?
C1A C2A 1.449(4) . ?
C1A C5A 1.461(4) . ?
C1A C6A 1.488(4) . ?
C6A H6A1 0.9800 . ?
C6A H6A2 0.9800 . ?
C6A H6A3 0.9800 . ?
C2A C7A 1.498(4) . ?
C4A C5A 1.410(4) . ?
C10A C5A 1.490(4) . ?
C10A H10A 0.9800 . ?
C10A H10B 0.9800 . ?
C10A H10C 0.9800 . ?
C7A H7A1 0.9800 . ?
C7A H7A2 0.9800 . ?
C7A H7A3 0.9800 . ?
C8A H8A1 0.9800 . ?
C8A H8A2 0.9800 . ?
C8A H8A3 0.9800 . ?
C1E H1E1 0.9900 . ?
C1E H1E2 0.9900 . ?
N2B N1B 1.324(3) . ?
N2B N3B 1.334(3) . ?
N3B C1B 1.350(3) . ?
N3B C7B 1.472(3) . ?
N1B C2B 1.356(3) . ?
N5B C6B 1.362(3) . ?
N5B C5B 1.389(3) . ?
N5B C14B 1.451(3) . ?
N4B C6B 1.361(3) . ?
N4B C4B 1.379(3) . ?
N4B C3B 1.468(3) . ?
C3B C2B 1.491(3) . ?
C3B H3B1 0.9900 . ?
C3B H3B2 0.9900 . ?
C2B C1B 1.363(4) . ?
C1B H1B 0.9500 . ?
C4B C5B 1.334(4) . ?
C4B H4B 0.9500 . ?
C5B H5B 0.9500 . ?
C14B C19B 1.393(4) . ?
C14B C15B 1.396(4) . ?
C19B C18B 1.391(4) . ?
C19B C22B 1.505(4) . ?
C18B C17B 1.382(4) . ?
C18B H18B 0.9500 . ?
C17B C16B 1.391(4) . ?
C17B C21B 1.513(4) . ?
C8B C9B 1.383(4) . ?
C8B C13B 1.384(4) . ?
C8B C7B 1.503(4) . ?
C7B H7B1 0.9900 . ?
C7B H7B2 0.9900 . ?
C16B C15B 1.391(4) . ?
C16B H16B 0.9500 . ?
C15B C20B 1.502(4) . ?
C20B H20A 0.9800 . ?
C20B H20B 0.9800 . ?
C20B H20C 0.9800 . ?
C9B C10B 1.389(5) . ?
C9B H9B 0.9500 . ?
C22B H22A 0.9800 . ?
C22B H22B 0.9800 . ?
C22B H22D 0.9800 . ?
C10B C11B 1.365(6) . ?
C10B H10D 0.9500 . ?
C12B C11B 1.368(6) . ?
C12B C13B 1.386(5) . ?
C12B H12B 0.9500 . ?
C13B H13B 0.9500 . ?
C21B H21A 0.9800 . ?
C21B H21B 0.9800 . ?
C21B H21C 0.9800 . ?
C11B H11B 0.9500 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6B Ir1 N1B 83.29(9) . . ?
C6B Ir1 C1A 111.59(10) . . ?
N1B Ir1 C1A 160.65(9) . . ?
C6B Ir1 C3A 119.19(10) . . ?
N1B Ir1 C3A 97.31(9) . . ?
C1A Ir1 C3A 64.99(10) . . ?
C6B Ir1 C2A 98.47(10) . . ?
N1B Ir1 C2A 129.46(9) . . ?
C1A Ir1 C2A 39.01(10) . . ?
C3A Ir1 C2A 38.31(10) . . ?
C6B Ir1 C4A 157.69(10) . . ?
N1B Ir1 C4A 97.14(8) . . ?
C1A Ir1 C4A 64.32(9) . . ?
C3A Ir1 C4A 38.52(10) . . ?
C2A Ir1 C4A 64.03(10) . . ?
C6B Ir1 C5A 149.15(10) . . ?
N1B Ir1 C5A 127.55(9) . . ?
C1A Ir1 C5A 38.87(9) . . ?
C3A Ir1 C5A 63.51(10) . . ?
C2A Ir1 C5A 64.04(10) . . ?
C4A Ir1 C5A 36.99(10) . . ?
C6B Ir1 Cl2 90.03(7) . . ?
N1B Ir1 Cl2 86.97(6) . . ?
C1A Ir1 Cl2 104.70(7) . . ?
C3A Ir1 Cl2 150.75(7) . . ?
C2A Ir1 Cl2 143.19(7) . . ?
C4A Ir1 Cl2 112.28(7) . . ?
C5A Ir1 Cl2 90.96(7) . . ?
C31C B1C C21C 109.1(2) . . ?
C31C B1C C11C 107.8(2) . . ?
C21C B1C C11C 110.7(2) . . ?
C31C B1C C41C 109.8(2) . . ?
C21C B1C C41C 110.3(2) . . ?
C11C B1C C41C 109.1(2) . . ?
C16C C11C C12C 114.8(3) . . ?
C16C C11C B1C 125.3(2) . . ?
C12C C11C B1C 119.8(2) . . ?
C11C C16C C15C 122.3(3) . . ?
C11C C16C H16C 118.8 . . ?
C15C C16C H16C 118.9 . . ?
C14C C13C C12C 119.9(3) . . ?
C14C C13C H13C 120.0 . . ?
C12C C13C H13C 120.0 . . ?
C13C C12C C11C 123.5(3) . . ?
C13C C12C H12C 118.2 . . ?
C11C C12C H12C 118.2 . . ?
C14C C15C C16C 120.5(3) . . ?
C14C C15C H15C 119.8 . . ?
C16C C15C H15C 119.8 . . ?
C13C C14C C15C 118.9(3) . . ?
C13C C14C H14C 120.5 . . ?
C15C C14C H14C 120.5 . . ?
C26C C21C C22C 114.3(2) . . ?
C26C C21C B1C 124.4(2) . . ?
C22C C21C B1C 121.2(2) . . ?
C25C C26C C21C 122.9(2) . . ?
C25C C26C H26C 118.6 . . ?
C21C C26C H26C 118.6 . . ?
C23C C22C C21C 123.2(2) . . ?
C23C C22C H22C 118.4 . . ?
C21C C22C H22C 118.4 . . ?
C24C C23C C22C 120.2(3) . . ?
C24C C23C H23C 119.9 . . ?
C22C C23C H23C 119.9 . . ?
C24C C25C C26C 120.6(3) . . ?
C24C C25C H25C 119.7 . . ?
C26C C25C H25C 119.7 . . ?
C25C C24C C23C 118.6(3) . . ?
C25C C24C H24C 120.7 . . ?
C23C C24C H24C 120.7 . . ?
C35C C34C C33C 118.8(2) . . ?
C35C C34C H34C 120.6 . . ?
C33C C34C H34C 120.6 . . ?
C33C C32C C31C 123.3(2) . . ?
C33C C32C H32C 118.4 . . ?
C31C C32C H32C 118.4 . . ?
C36C C31C C32C 114.8(2) . . ?
C36C C31C B1C 125.2(2) . . ?
C32C C31C B1C 120.0(2) . . ?
C35C C36C C31C 122.9(2) . . ?
C35C C36C H36C 118.6 . . ?
C31C C36C H36C 118.6 . . ?
C32C C33C C34C 120.0(2) . . ?
C32C C33C H33C 120.0 . . ?
C34C C33C H33C 120.0 . . ?
C34C C35C C36C 120.2(2) . . ?
C34C C35C H35C 119.9 . . ?
C36C C35C H35C 119.9 . . ?
C46C C41C C42C 114.6(2) . . ?
C46C C41C B1C 122.7(2) . . ?
C42C C41C B1C 122.7(2) . . ?
C43C C42C C41C 123.0(3) . . ?
C43C C42C H42C 118.5 . . ?
C41C C42C H42C 118.5 . . ?
C45C C46C C41C 123.0(3) . . ?
C45C C46C H46C 118.5 . . ?
C41C C46C H46C 118.5 . . ?
C44C C43C C42C 120.2(3) . . ?
C44C C43C H43C 119.9 . . ?
C42C C43C H43C 119.9 . . ?
C44C C45C C46C 120.2(3) . . ?
C44C C45C H45C 119.9 . . ?
C46C C45C H45C 119.9 . . ?
C43C C44C C45C 118.9(3) . . ?
C43C C44C H44C 120.6 . . ?
C45C C44C H44C 120.6 . . ?
Cl2D C1D Cl1D 112.3(2) . . ?
Cl2D C1D H1D1 109.2 . . ?
Cl1D C1D H1D1 109.2 . . ?
Cl2D C1D H1D2 109.2 . . ?
Cl1D C1D H1D2 109.2 . . ?
H1D1 C1D H1D2 107.9 . . ?
C4A C9A H9A1 109.5 . . ?
C4A C9A H9A2 109.5 . . ?
H9A1 C9A H9A2 109.5 . . ?
C4A C9A H9A3 109.5 . . ?
H9A1 C9A H9A3 109.5 . . ?
H9A2 C9A H9A3 109.5 . . ?
C2A C3A C4A 108.3(2) . . ?
C2A C3A C8A 126.2(2) . . ?
C4A C3A C8A 124.8(2) . . ?
C2A C3A Ir1 71.00(14) . . ?
C4A C3A Ir1 72.71(14) . . ?
C8A C3A Ir1 129.39(18) . . ?
C2A C1A C5A 106.5(2) . . ?
C2A C1A C6A 127.8(2) . . ?
C5A C1A C6A 124.9(2) . . ?
C2A C1A Ir1 70.79(14) . . ?
C5A C1A Ir1 72.67(13) . . ?
C6A C1A Ir1 129.68(19) . . ?
C1A C6A H6A1 109.5 . . ?
C1A C6A H6A2 109.5 . . ?
H6A1 C6A H6A2 109.5 . . ?
C1A C6A H6A3 109.5 . . ?
H6A1 C6A H6A3 109.5 . . ?
H6A2 C6A H6A3 109.5 . . ?
C3A C2A C1A 108.3(2) . . ?
C3A C2A C7A 124.3(2) . . ?
C1A C2A C7A 127.3(2) . . ?
C3A C2A Ir1 70.69(14) . . ?
C1A C2A Ir1 70.19(14) . . ?
C7A C2A Ir1 128.15(19) . . ?
C5A C4A C3A 107.9(2) . . ?
C5A C4A C9A 127.2(3) . . ?
C3A C4A C9A 124.8(2) . . ?
C5A C4A Ir1 71.51(14) . . ?
C3A C4A Ir1 68.77(13) . . ?
C9A C4A Ir1 128.15(18) . . ?
C5A C10A H10A 109.5 . . ?
C5A C10A H10B 109.5 . . ?
H10A C10A H10B 109.5 . . ?
C5A C10A H10C 109.5 . . ?
H10A C10A H10C 109.5 . . ?
H10B C10A H10C 109.5 . . ?
C4A C5A C1A 108.9(2) . . ?
C4A C5A C10A 126.3(2) . . ?
C1A C5A C10A 124.8(2) . . ?
C4A C5A Ir1 71.50(14) . . ?
C1A C5A Ir1 68.46(13) . . ?
C10A C5A Ir1 125.34(18) . . ?
C2A C7A H7A1 109.5 . . ?
C2A C7A H7A2 109.5 . . ?
H7A1 C7A H7A2 109.5 . . ?
C2A C7A H7A3 109.5 . . ?
H7A1 C7A H7A3 109.5 . . ?
H7A2 C7A H7A3 109.5 . . ?
C3A C8A H8A1 109.5 . . ?
C3A C8A H8A2 109.5 . . ?
H8A1 C8A H8A2 109.5 . . ?
C3A C8A H8A3 109.5 . . ?
H8A1 C8A H8A3 109.5 . . ?
H8A2 C8A H8A3 109.5 . . ?
Cl1E C1E Cl2E 111.04(18) . . ?
Cl1E C1E H1E1 109.4 . . ?
Cl2E C1E H1E1 109.4 . . ?
Cl1E C1E H1E2 109.4 . . ?
Cl2E C1E H1E2 109.4 . . ?
H1E1 C1E H1E2 108.0 . . ?
N1B N2B N3B 105.23(19) . . ?
N2B N3B C1B 112.0(2) . . ?
N2B N3B C7B 120.0(2) . . ?
C1B N3B C7B 128.0(2) . . ?
N2B N1B C2B 110.6(2) . . ?
N2B N1B Ir1 126.20(16) . . ?
C2B N1B Ir1 123.09(16) . . ?
C6B N5B C5B 110.4(2) . . ?
C6B N5B C14B 130.0(2) . . ?
C5B N5B C14B 119.5(2) . . ?
C6B N4B C4B 112.3(2) . . ?
C6B N4B C3B 123.4(2) . . ?
C4B N4B C3B 124.2(2) . . ?
N4B C3B C2B 109.4(2) . . ?
N4B C3B H3B1 109.8 . . ?
C2B C3B H3B1 109.8 . . ?
N4B C3B H3B2 109.8 . . ?
C2B C3B H3B2 109.8 . . ?
H3B1 C3B H3B2 108.2 . . ?
N1B C2B C1B 107.2(2) . . ?
N1B C2B C3B 119.3(2) . . ?
C1B C2B C3B 133.6(2) . . ?
N4B C6B N5B 103.5(2) . . ?
N4B C6B Ir1 120.59(18) . . ?
N5B C6B Ir1 135.79(19) . . ?
N3B C1B C2B 105.0(2) . . ?
N3B C1B H1B 127.5 . . ?
C2B C1B H1B 127.5 . . ?
C5B C4B N4B 105.9(2) . . ?
C5B C4B H4B 127.1 . . ?
N4B C4B H4B 127.1 . . ?
C4B C5B N5B 107.9(2) . . ?
C4B C5B H5B 126.0 . . ?
N5B C5B H5B 126.0 . . ?
C19B C14B C15B 122.0(2) . . ?
C19B C14B N5B 118.5(2) . . ?
C15B C14B N5B 118.8(2) . . ?
C18B C19B C14B 117.8(2) . . ?
C18B C19B C22B 119.3(3) . . ?
C14B C19B C22B 122.6(3) . . ?
C17B C18B C19B 122.0(3) . . ?
C17B C18B H18B 119.0 . . ?
C19B C18B H18B 119.0 . . ?
C18B C17B C16B 118.2(2) . . ?
C18B C17B C21B 120.9(3) . . ?
C16B C17B C21B 120.9(3) . . ?
C9B C8B C13B 118.9(3) . . ?
C9B C8B C7B 120.0(3) . . ?
C13B C8B C7B 121.1(3) . . ?
N3B C7B C8B 113.0(2) . . ?
N3B C7B H7B1 109.0 . . ?
C8B C7B H7B1 109.0 . . ?
N3B C7B H7B2 109.0 . . ?
C8B C7B H7B2 109.0 . . ?
H7B1 C7B H7B2 107.8 . . ?
C15B C16B C17B 122.1(3) . . ?
C15B C16B H16B 118.9 . . ?
C17B C16B H16B 118.9 . . ?
C16B C15B C14B 117.4(2) . . ?
C16B C15B C20B 120.2(3) . . ?
C14B C15B C20B 122.3(3) . . ?
C15B C20B H20A 109.5 . . ?
C15B C20B H20B 109.5 . . ?
H20A C20B H20B 109.5 . . ?
C15B C20B H20C 109.5 . . ?
H20A C20B H20C 109.5 . . ?
H20B C20B H20C 109.5 . . ?
C8B C9B C10B 120.1(3) . . ?
C8B C9B H9B 119.9 . . ?
C10B C9B H9B 119.9 . . ?
C19B C22B H22A 109.5 . . ?
C19B C22B H22B 109.5 . . ?
H22A C22B H22B 109.5 . . ?
C19B C22B H22D 109.5 . . ?
H22A C22B H22D 109.5 . . ?
H22B C22B H22D 109.5 . . ?
C11B C10B C9B 120.4(4) . . ?
C11B C10B H10D 119.8 . . ?
C9B C10B H10D 119.8 . . ?
C11B C12B C13B 120.1(4) . . ?
C11B C12B H12B 119.9 . . ?
C13B C12B H12B 119.9 . . ?
C8B C13B C12B 120.4(3) . . ?
C8B C13B H13B 119.8 . . ?
C12B C13B H13B 119.8 . . ?
C17B C21B H21A 109.5 . . ?
C17B C21B H21B 109.5 . . ?
H21A C21B H21B 109.5 . . ?
C17B C21B H21C 109.5 . . ?
H21A C21B H21C 109.5 . . ?
H21B C21B H21C 109.5 . . ?
C10B C11B C12B 120.1(3) . . ?
C10B C11B H11B 120.0 . . ?
C12B C11B H11B 120.0 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C31C B1C C11C C16C -141.4(2) . . . . ?
C21C B1C C11C C16C -22.1(3) . . . . ?
C41C B1C C11C C16C 99.5(3) . . . . ?
C31C B1C C11C C12C 40.3(3) . . . . ?
C21C B1C C11C C12C 159.6(2) . . . . ?
C41C B1C C11C C12C -78.9(3) . . . . ?
C12C C11C C16C C15C -1.1(4) . . . . ?
B1C C11C C16C C15C -179.4(2) . . . . ?
C14C C13C C12C C11C 0.7(5) . . . . ?
C16C C11C C12C C13C 0.3(4) . . . . ?
B1C C11C C12C C13C 178.8(3) . . . . ?
C11C C16C C15C C14C 0.9(4) . . . . ?
C12C C13C C14C C15C -0.9(5) . . . . ?
C16C C15C C14C C13C 0.2(5) . . . . ?
C31C B1C C21C C26C 6.8(3) . . . . ?
C11C B1C C21C C26C -111.7(3) . . . . ?
C41C B1C C21C C26C 127.5(3) . . . . ?
C31C B1C C21C C22C -174.9(2) . . . . ?
C11C B1C C21C C22C 66.6(3) . . . . ?
C41C B1C C21C C22C -54.2(3) . . . . ?
C22C C21C C26C C25C -2.8(4) . . . . ?
B1C C21C C26C C25C 175.6(2) . . . . ?
C26C C21C C22C C23C 3.6(4) . . . . ?
B1C C21C C22C C23C -174.8(3) . . . . ?
C21C C22C C23C C24C -2.1(4) . . . . ?
C21C C26C C25C C24C 0.4(4) . . . . ?
C26C C25C C24C C23C 1.4(4) . . . . ?
C22C C23C C24C C25C -0.6(4) . . . . ?
C33C C32C C31C C36C -2.5(4) . . . . ?
C33C C32C C31C B1C 175.5(2) . . . . ?
C21C B1C C31C C36C 113.8(3) . . . . ?
C11C B1C C31C C36C -125.9(3) . . . . ?
C41C B1C C31C C36C -7.2(3) . . . . ?
C21C B1C C31C C32C -64.0(3) . . . . ?
C11C B1C C31C C32C 56.3(3) . . . . ?
C41C B1C C31C C32C 175.1(2) . . . . ?
C32C C31C C36C C35C 2.1(4) . . . . ?
B1C C31C C36C C35C -175.8(2) . . . . ?
C31C C32C C33C C34C 1.3(4) . . . . ?
C35C C34C C33C C32C 0.3(4) . . . . ?
C33C C34C C35C C36C -0.7(4) . . . . ?
C31C C36C C35C C34C -0.6(4) . . . . ?
C31C B1C C41C C46C -81.8(3) . . . . ?
C21C B1C C41C C46C 157.9(2) . . . . ?
C11C B1C C41C C46C 36.2(3) . . . . ?
C31C B1C C41C C42C 96.0(3) . . . . ?
C21C B1C C41C C42C -24.2(3) . . . . ?
C11C B1C C41C C42C -146.0(2) . . . . ?
C46C C41C C42C C43C 0.4(4) . . . . ?
B1C C41C C42C C43C -177.6(2) . . . . ?
C42C C41C C46C C45C -0.2(4) . . . . ?
B1C C41C C46C C45C 177.8(2) . . . . ?
C41C C42C C43C C44C -0.1(4) . . . . ?
C41C C46C C45C C44C -0.3(4) . . . . ?
C42C C43C C44C C45C -0.3(4) . . . . ?
C46C C45C C44C C43C 0.5(4) . . . . ?
C6B Ir1 C3A C2A 64.22(18) . . . . ?
N1B Ir1 C3A C2A 150.60(15) . . . . ?
C1A Ir1 C3A C2A -37.58(15) . . . . ?
C4A Ir1 C3A C2A -117.1(2) . . . . ?
C5A Ir1 C3A C2A -80.90(16) . . . . ?
Cl2 Ir1 C3A C2A -112.52(17) . . . . ?
C6B Ir1 C3A C4A -178.67(14) . . . . ?
N1B Ir1 C3A C4A -92.29(15) . . . . ?
C1A Ir1 C3A C4A 79.54(16) . . . . ?
C2A Ir1 C3A C4A 117.1(2) . . . . ?
C5A Ir1 C3A C4A 36.21(14) . . . . ?
Cl2 Ir1 C3A C4A 4.6(2) . . . . ?
C6B Ir1 C3A C8A -57.5(3) . . . . ?
N1B Ir1 C3A C8A 28.9(3) . . . . ?
C1A Ir1 C3A C8A -159.3(3) . . . . ?
C2A Ir1 C3A C8A -121.7(3) . . . . ?
C4A Ir1 C3A C8A 121.2(3) . . . . ?
C5A Ir1 C3A C8A 157.4(3) . . . . ?
Cl2 Ir1 C3A C8A 125.8(2) . . . . ?
C6B Ir1 C1A C2A -76.30(16) . . . . ?
N1B Ir1 C1A C2A 62.1(3) . . . . ?
C3A Ir1 C1A C2A 36.91(15) . . . . ?
C4A Ir1 C1A C2A 79.72(16) . . . . ?
C5A Ir1 C1A C2A 115.0(2) . . . . ?
Cl2 Ir1 C1A C2A -172.29(13) . . . . ?
C6B Ir1 C1A C5A 168.65(15) . . . . ?
N1B Ir1 C1A C5A -53.0(3) . . . . ?
C3A Ir1 C1A C5A -78.14(16) . . . . ?
C2A Ir1 C1A C5A -115.0(2) . . . . ?
C4A Ir1 C1A C5A -35.33(15) . . . . ?
Cl2 Ir1 C1A C5A 72.66(15) . . . . ?
C6B Ir1 C1A C6A 47.3(3) . . . . ?
N1B Ir1 C1A C6A -174.3(2) . . . . ?
C3A Ir1 C1A C6A 160.5(3) . . . . ?
C2A Ir1 C1A C6A 123.6(3) . . . . ?
C4A Ir1 C1A C6A -156.7(3) . . . . ?
C5A Ir1 C1A C6A -121.3(3) . . . . ?
Cl2 Ir1 C1A C6A -48.7(2) . . . . ?
C4A C3A C2A C1A -3.1(3) . . . . ?
C8A C3A C2A C1A -174.1(2) . . . . ?
Ir1 C3A C2A C1A 60.42(17) . . . . ?
C4A C3A C2A C7A 172.9(2) . . . . ?
C8A C3A C2A C7A 1.8(4) . . . . ?
Ir1 C3A C2A C7A -123.6(3) . . . . ?
C4A C3A C2A Ir1 -63.55(17) . . . . ?
C8A C3A C2A Ir1 125.4(3) . . . . ?
C5A C1A C2A C3A 3.7(3) . . . . ?
C6A C1A C2A C3A 173.4(2) . . . . ?
Ir1 C1A C2A C3A -60.74(17) . . . . ?
C5A C1A C2A C7A -172.2(2) . . . . ?
C6A C1A C2A C7A -2.4(4) . . . . ?
Ir1 C1A C2A C7A 123.4(3) . . . . ?
C5A C1A C2A Ir1 64.41(16) . . . . ?
C6A C1A C2A Ir1 -125.8(3) . . . . ?
C6B Ir1 C2A C3A -127.36(16) . . . . ?
N1B Ir1 C2A C3A -39.10(19) . . . . ?
C1A Ir1 C2A C3A 118.6(2) . . . . ?
C4A Ir1 C2A C3A 38.07(15) . . . . ?
C5A Ir1 C2A C3A 79.39(16) . . . . ?
Cl2 Ir1 C2A C3A 131.12(14) . . . . ?
C6B Ir1 C2A C1A 114.02(15) . . . . ?
N1B Ir1 C2A C1A -157.72(13) . . . . ?
C3A Ir1 C2A C1A -118.6(2) . . . . ?
C4A Ir1 C2A C1A -80.54(16) . . . . ?
C5A Ir1 C2A C1A -39.22(14) . . . . ?
Cl2 Ir1 C2A C1A 12.5(2) . . . . ?
C6B Ir1 C2A C7A -8.4(3) . . . . ?
N1B Ir1 C2A C7A 79.9(3) . . . . ?
C1A Ir1 C2A C7A -122.4(3) . . . . ?
C3A Ir1 C2A C7A 119.0(3) . . . . ?
C4A Ir1 C2A C7A 157.1(3) . . . . ?
C5A Ir1 C2A C7A -161.6(3) . . . . ?
Cl2 Ir1 C2A C7A -109.9(2) . . . . ?
C2A C3A C4A C5A 1.3(3) . . . . ?
C8A C3A C4A C5A 172.5(2) . . . . ?
Ir1 C3A C4A C5A -61.13(17) . . . . ?
C2A C3A C4A C9A -175.1(2) . . . . ?
C8A C3A C4A C9A -3.9(4) . . . . ?
Ir1 C3A C4A C9A 122.5(2) . . . . ?
C2A C3A C4A Ir1 62.46(17) . . . . ?
C8A C3A C4A Ir1 -126.4(3) . . . . ?
C6B Ir1 C4A C5A 121.6(3) . . . . ?
N1B Ir1 C4A C5A -148.71(15) . . . . ?
C1A Ir1 C4A C5A 37.09(15) . . . . ?
C3A Ir1 C4A C5A 118.5(2) . . . . ?
C2A Ir1 C4A C5A 80.64(16) . . . . ?
Cl2 Ir1 C4A C5A -59.07(15) . . . . ?
C6B Ir1 C4A C3A 3.1(3) . . . . ?
N1B Ir1 C4A C3A 92.79(15) . . . . ?
C1A Ir1 C4A C3A -81.41(16) . . . . ?
C2A Ir1 C4A C3A -37.86(15) . . . . ?
C5A Ir1 C4A C3A -118.5(2) . . . . ?
Cl2 Ir1 C4A C3A -177.58(12) . . . . ?
C6B Ir1 C4A C9A -115.2(3) . . . . ?
N1B Ir1 C4A C9A -25.5(3) . . . . ?
C1A Ir1 C4A C9A 160.3(3) . . . . ?
C3A Ir1 C4A C9A -118.2(3) . . . . ?
C2A Ir1 C4A C9A -156.1(3) . . . . ?
C5A Ir1 C4A C9A 123.2(3) . . . . ?
Cl2 Ir1 C4A C9A 64.2(3) . . . . ?
C3A C4A C5A C1A 1.0(3) . . . . ?
C9A C4A C5A C1A 177.3(2) . . . . ?
Ir1 C4A C5A C1A -58.40(17) . . . . ?
C3A C4A C5A C10A -179.9(2) . . . . ?
C9A C4A C5A C10A -3.6(4) . . . . ?
Ir1 C4A C5A C10A 120.7(3) . . . . ?
C3A C4A C5A Ir1 59.40(16) . . . . ?
C9A C4A C5A Ir1 -124.3(3) . . . . ?
C2A C1A C5A C4A -2.9(3) . . . . ?
C6A C1A C5A C4A -173.0(2) . . . . ?
Ir1 C1A C5A C4A 60.27(17) . . . . ?
C2A C1A C5A C10A 178.0(2) . . . . ?
C6A C1A C5A C10A 7.8(4) . . . . ?
Ir1 C1A C5A C10A -118.9(2) . . . . ?
C2A C1A C5A Ir1 -63.15(16) . . . . ?
C6A C1A C5A Ir1 126.7(3) . . . . ?
C6B Ir1 C5A C4A -140.89(19) . . . . ?
N1B Ir1 C5A C4A 40.54(19) . . . . ?
C1A Ir1 C5A C4A -120.0(2) . . . . ?
C3A Ir1 C5A C4A -37.70(15) . . . . ?
C2A Ir1 C5A C4A -80.61(16) . . . . ?
Cl2 Ir1 C5A C4A 127.45(14) . . . . ?
C6B Ir1 C5A C1A -20.9(3) . . . . ?
N1B Ir1 C5A C1A 160.52(14) . . . . ?
C3A Ir1 C5A C1A 82.28(16) . . . . ?
C2A Ir1 C5A C1A 39.37(15) . . . . ?
C4A Ir1 C5A C1A 120.0(2) . . . . ?
Cl2 Ir1 C5A C1A -112.57(14) . . . . ?
C6B Ir1 C5A C10A 97.2(3) . . . . ?
N1B Ir1 C5A C10A -81.3(2) . . . . ?
C1A Ir1 C5A C10A 118.1(3) . . . . ?
C3A Ir1 C5A C10A -159.6(3) . . . . ?
C2A Ir1 C5A C10A 157.5(3) . . . . ?
C4A Ir1 C5A C10A -121.9(3) . . . . ?
Cl2 Ir1 C5A C10A 5.6(2) . . . . ?
N1B N2B N3B C1B -0.6(3) . . . . ?
N1B N2B N3B C7B -178.6(2) . . . . ?
N3B N2B N1B C2B 0.5(2) . . . . ?
N3B N2B N1B Ir1 -176.69(15) . . . . ?
C6B Ir1 N1B N2B -140.8(2) . . . . ?
C1A Ir1 N1B N2B 77.7(3) . . . . ?
C3A Ir1 N1B N2B 100.54(19) . . . . ?
C2A Ir1 N1B N2B 123.76(19) . . . . ?
C4A Ir1 N1B N2B 61.7(2) . . . . ?
C5A Ir1 N1B N2B 38.5(2) . . . . ?
Cl2 Ir1 N1B N2B -50.39(18) . . . . ?
C6B Ir1 N1B C2B 42.41(19) . . . . ?
C1A Ir1 N1B C2B -99.1(3) . . . . ?
C3A Ir1 N1B C2B -76.27(19) . . . . ?
C2A Ir1 N1B C2B -53.1(2) . . . . ?
C4A Ir1 N1B C2B -115.11(19) . . . . ?
C5A Ir1 N1B C2B -138.32(18) . . . . ?
Cl2 Ir1 N1B C2B 132.80(18) . . . . ?
C6B N4B C3B C2B 54.8(3) . . . . ?
C4B N4B C3B C2B -121.0(3) . . . . ?
N2B N1B C2B C1B -0.1(3) . . . . ?
Ir1 N1B C2B C1B 177.11(16) . . . . ?
N2B N1B C2B C3B 179.0(2) . . . . ?
Ir1 N1B C2B C3B -3.7(3) . . . . ?
N4B C3B C2B N1B -51.3(3) . . . . ?
N4B C3B C2B C1B 127.6(3) . . . . ?
C4B N4B C6B N5B -0.6(3) . . . . ?
C3B N4B C6B N5B -176.9(2) . . . . ?
C4B N4B C6B Ir1 176.41(19) . . . . ?
C3B N4B C6B Ir1 0.1(3) . . . . ?
C5B N5B C6B N4B 0.5(3) . . . . ?
C14B N5B C6B N4B -177.3(3) . . . . ?
C5B N5B C6B Ir1 -175.8(2) . . . . ?
C14B N5B C6B Ir1 6.5(5) . . . . ?
N1B Ir1 C6B N4B -39.8(2) . . . . ?
C1A Ir1 C6B N4B 127.4(2) . . . . ?
C3A Ir1 C6B N4B 54.8(2) . . . . ?
C2A Ir1 C6B N4B 89.2(2) . . . . ?
C4A Ir1 C6B N4B 52.7(4) . . . . ?
C5A Ir1 C6B N4B 141.3(2) . . . . ?
Cl2 Ir1 C6B N4B -126.75(19) . . . . ?
N1B Ir1 C6B N5B 136.0(3) . . . . ?
C1A Ir1 C6B N5B -56.8(3) . . . . ?
C3A Ir1 C6B N5B -129.4(3) . . . . ?
C2A Ir1 C6B N5B -95.0(3) . . . . ?
C4A Ir1 C6B N5B -131.5(3) . . . . ?
C5A Ir1 C6B N5B -42.9(4) . . . . ?
Cl2 Ir1 C6B N5B 49.1(3) . . . . ?
N2B N3B C1B C2B 0.5(3) . . . . ?
C7B N3B C1B C2B 178.3(2) . . . . ?
N1B C2B C1B N3B -0.2(3) . . . . ?
C3B C2B C1B N3B -179.2(3) . . . . ?
C6B N4B C4B C5B 0.5(3) . . . . ?
C3B N4B C4B C5B 176.7(3) . . . . ?
N4B C4B C5B N5B -0.2(4) . . . . ?
C6B N5B C5B C4B -0.2(4) . . . . ?
C14B N5B C5B C4B 177.8(3) . . . . ?
C6B N5B C14B C19B 89.8(3) . . . . ?
C5B N5B C14B C19B -87.7(3) . . . . ?
C6B N5B C14B C15B -99.5(3) . . . . ?
C5B N5B C14B C15B 82.9(3) . . . . ?
C15B C14B C19B C18B 7.3(4) . . . . ?
N5B C14B C19B C18B 177.6(2) . . . . ?
C15B C14B C19B C22B -167.3(3) . . . . ?
N5B C14B C19B C22B 3.0(4) . . . . ?
C14B C19B C18B C17B -3.2(4) . . . . ?
C22B C19B C18B C17B 171.7(3) . . . . ?
C19B C18B C17B C16B -1.5(4) . . . . ?
C19B C18B C17B C21B -179.4(3) . . . . ?
N2B N3B C7B C8B 91.3(3) . . . . ?
C1B N3B C7B C8B -86.3(3) . . . . ?
C9B C8B C7B N3B -116.2(3) . . . . ?
C13B C8B C7B N3B 65.6(3) . . . . ?
C18B C17B C16B C15B 2.5(4) . . . . ?
C21B C17B C16B C15B -179.6(3) . . . . ?
C17B C16B C15B C14B 1.4(4) . . . . ?
C17B C16B C15B C20B -175.2(2) . . . . ?
C19B C14B C15B C16B -6.4(4) . . . . ?
N5B C14B C15B C16B -176.7(2) . . . . ?
C19B C14B C15B C20B 170.1(2) . . . . ?
N5B C14B C15B C20B -0.2(4) . . . . ?
C13B C8B C9B C10B -0.2(4) . . . . ?
C7B C8B C9B C10B -178.6(3) . . . . ?
C8B C9B C10B C11B -1.4(5) . . . . ?
C9B C8B C13B C12B 1.4(4) . . . . ?
C7B C8B C13B C12B 179.7(3) . . . . ?
C11B C12B C13B C8B -0.9(5) . . . . ?
C9B C10B C11B C12B 1.9(5) . . . . ?
C13B C12B C11B C10B -0.8(5) . . . . ?
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full 24.99
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max 1.024
_refine_diff_density_min -0.819
_refine_diff_density_rms 0.066
_database_code_depnum_ccdc_archive 'CCDC 934042'
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_marina2_rhodium
#TrackingRef 'Marina2_Deposition_16June11.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C32 H38 Cl N5 Rh, C24 H20 B, 2(C H2 Cl2)'
_chemical_formula_sum 'C58 H62 B Cl5 N5 Rh'
_chemical_formula_weight 1120.10
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Triclinic
_symmetry_space_group_name_H-M P-1
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 13.4167(5)
_cell_length_b 13.6538(5)
_cell_length_c 14.7446(5)
_cell_angle_alpha 89.616(2)
_cell_angle_beta 83.727(2)
_cell_angle_gamma 85.346(2)
_cell_volume 2676.02(17)
_cell_formula_units_Z 2
_cell_measurement_temperature 155(2)
_cell_measurement_reflns_used 9916
_cell_measurement_theta_min 3.024
_cell_measurement_theta_max 30.320
_exptl_crystal_description Block
_exptl_crystal_colour Orange
_exptl_crystal_size_max 0.36
_exptl_crystal_size_mid 0.22
_exptl_crystal_size_min 0.09
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.390
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1160
_exptl_absorpt_coefficient_mu 0.612
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.8079
_exptl_absorpt_correction_T_max 0.9475
_exptl_absorpt_process_details 'SADABS (Bruker, 2001)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 155(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker kappa APEXII CCD Diffractometer'
_diffrn_measurement_method '\f scans, and \w scans with \k offsets'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 28228
_diffrn_reflns_av_R_equivalents 0.0341
_diffrn_reflns_av_sigmaI/netI 0.0337
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_theta_min 1.50
_diffrn_reflns_theta_max 25.00
_reflns_number_total 9163
_reflns_number_gt 8012
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2007)'
_computing_cell_refinement 'APEX2 (Bruker, 2007)'
_computing_data_reduction 'APEX2 (Bruker, 2007)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
Final difference Fourier revealed two peaks ~ 0.75 eA-3 near chlorides Cl1D
and Cl2D, which implies orientational disorder of the solvent molecule,
Dichloromethane. However, this position due to low peak heights
(therefore low occupancy) was not included in the least-squares refinement.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0341P)^2^+3.1579P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 9163
_refine_ls_number_parameters 639
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0405
_refine_ls_R_factor_gt 0.0325
_refine_ls_wR_factor_ref 0.0854
_refine_ls_wR_factor_gt 0.0801
_refine_ls_goodness_of_fit_ref 1.052
_refine_ls_restrained_S_all 1.052
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.780243(14) 0.763572(13) 0.734879(13) 0.01657(7) Uani 1 1 d . . .
Cl1 Cl 0.80131(5) 0.72389(5) 0.88923(4) 0.02673(15) Uani 1 1 d . . .
C1A C 0.94573(18) 0.75501(19) 0.70116(18) 0.0225(5) Uani 1 1 d . . .
C2A C 0.90487(19) 0.69608(19) 0.63865(18) 0.0240(6) Uani 1 1 d . . .
C3A C 0.83536(19) 0.75884(19) 0.59087(17) 0.0241(6) Uani 1 1 d . . .
C4A C 0.83556(19) 0.85676(19) 0.62340(18) 0.0245(6) Uani 1 1 d . . .
C5A C 0.90016(19) 0.85522(18) 0.69488(18) 0.0228(5) Uani 1 1 d . . .
C6A C 1.02140(19) 0.7216(2) 0.7639(2) 0.0296(6) Uani 1 1 d . . .
H6A1 H 1.0089 0.6553 0.7859 0.044 Uiso 1 1 calc R . .
H6A2 H 1.0159 0.7668 0.8159 0.044 Uiso 1 1 calc R . .
H6A3 H 1.0891 0.7207 0.7312 0.044 Uiso 1 1 calc R . .
C7A C 0.9318(2) 0.5893(2) 0.6195(2) 0.0342(7) Uani 1 1 d . . .
H7A1 H 0.9812 0.5818 0.5654 0.051 Uiso 1 1 calc R . .
H7A2 H 0.8713 0.5576 0.6085 0.051 Uiso 1 1 calc R . .
H7A3 H 0.9607 0.5585 0.6720 0.051 Uiso 1 1 calc R . .
C8A C 0.7851(2) 0.7263(2) 0.51153(19) 0.0335(7) Uani 1 1 d . . .
H8A1 H 0.7339 0.7776 0.4969 0.050 Uiso 1 1 calc R . .
H8A2 H 0.7532 0.6655 0.5273 0.050 Uiso 1 1 calc R . .
H8A3 H 0.8354 0.7147 0.4585 0.050 Uiso 1 1 calc R . .
C9A C 0.7819(2) 0.9445(2) 0.5836(2) 0.0341(7) Uani 1 1 d . . .
H9A1 H 0.8060 0.9498 0.5188 0.051 Uiso 1 1 calc R . .
H9A2 H 0.7950 1.0039 0.6157 0.051 Uiso 1 1 calc R . .
H9A3 H 0.7094 0.9371 0.5904 0.051 Uiso 1 1 calc R . .
C10A C 0.9307(2) 0.9415(2) 0.7445(2) 0.0313(6) Uani 1 1 d . . .
H10A H 0.9998 0.9542 0.7217 0.047 Uiso 1 1 calc R . .
H10C H 0.9269 0.9271 0.8100 0.047 Uiso 1 1 calc R . .
H10D H 0.8853 0.9995 0.7344 0.047 Uiso 1 1 calc R . .
N1B N 0.68539(15) 0.64795(14) 0.73277(14) 0.0182(4) Uani 1 1 d . . .
N2B N 0.70461(15) 0.55653(15) 0.75934(14) 0.0208(5) Uani 1 1 d . . .
N3B N 0.62475(16) 0.50971(15) 0.74238(14) 0.0213(5) Uani 1 1 d . . .
N4B N 0.56188(15) 0.83167(15) 0.73752(15) 0.0218(5) Uani 1 1 d . . .
N5B N 0.61617(16) 0.91825(16) 0.83953(16) 0.0287(5) Uani 1 1 d . . .
C1B C 0.55529(19) 0.56970(18) 0.70607(17) 0.0227(5) Uani 1 1 d . . .
H1B H 0.4925 0.5535 0.6887 0.027 Uiso 1 1 calc R . .
C2B C 0.59460(18) 0.65904(18) 0.69957(16) 0.0196(5) Uani 1 1 d . . .
C3B C 0.55690(19) 0.75753(18) 0.66704(18) 0.0223(5) Uani 1 1 d . . .
H3B1 H 0.5984 0.7750 0.6104 0.027 Uiso 1 1 calc R . .
H3B2 H 0.4865 0.7557 0.6532 0.027 Uiso 1 1 calc R . .
C4B C 0.4797(2) 0.8900(2) 0.7771(2) 0.0341(7) Uani 1 1 d . . .
H4B H 0.4125 0.8915 0.7621 0.041 Uiso 1 1 calc R . .
C5B C 0.5137(2) 0.9436(2) 0.8403(2) 0.0411(8) Uani 1 1 d . . .
H5B H 0.4748 0.9909 0.8792 0.049 Uiso 1 1 calc R . .
C6B C 0.64726(19) 0.84791(18) 0.77555(17) 0.0205(5) Uani 1 1 d . . .
C7B C 0.6200(2) 0.40462(18) 0.76613(19) 0.0265(6) Uani 1 1 d . . .
H7B1 H 0.6892 0.3728 0.7632 0.032 Uiso 1 1 calc R . .
H7B2 H 0.5846 0.3723 0.7206 0.032 Uiso 1 1 calc R . .
C8B C 0.5666(2) 0.38970(18) 0.85999(19) 0.0258(6) Uani 1 1 d . . .
C9B C 0.6191(3) 0.3474(2) 0.9278(2) 0.0427(8) Uani 1 1 d . . .
H9B H 0.6890 0.3287 0.9156 0.051 Uiso 1 1 calc R . .
C10B C 0.5694(4) 0.3322(3) 1.0138(3) 0.0636(12) Uani 1 1 d . . .
H10B H 0.6052 0.3019 1.0601 0.076 Uiso 1 1 calc R . .
C11B C 0.4697(4) 0.3606(3) 1.0322(3) 0.0670(13) Uani 1 1 d . . .
H11B H 0.4366 0.3513 1.0916 0.080 Uiso 1 1 calc R . .
C12B C 0.4171(3) 0.4020(2) 0.9661(3) 0.0588(11) Uani 1 1 d . . .
H12B H 0.3474 0.4215 0.9792 0.071 Uiso 1 1 calc R . .
C13B C 0.4651(2) 0.4158(2) 0.8799(2) 0.0418(8) Uani 1 1 d . . .
H13B H 0.4278 0.4437 0.8335 0.050 Uiso 1 1 calc R . .
C14B C 0.67368(19) 0.96821(19) 0.90011(19) 0.0251(6) Uani 1 1 d . . .
C15B C 0.7144(2) 1.0554(2) 0.87092(19) 0.0273(6) Uani 1 1 d . . .
C16B C 0.7663(2) 1.10378(19) 0.93153(19) 0.0281(6) Uani 1 1 d . . .
H16B H 0.7977 1.1613 0.9117 0.034 Uiso 1 1 calc R . .
C17B C 0.7737(2) 1.07096(19) 1.01941(19) 0.0284(6) Uani 1 1 d . . .
C18B C 0.7259(2) 0.98758(19) 1.04804(19) 0.0282(6) Uani 1 1 d . . .
H18B H 0.7288 0.9654 1.1090 0.034 Uiso 1 1 calc R . .
C19B C 0.6741(2) 0.93587(19) 0.9900(2) 0.0273(6) Uani 1 1 d . . .
C20B C 0.6168(2) 0.8505(2) 1.0254(2) 0.0399(8) Uani 1 1 d . . .
H20A H 0.5458 0.8634 1.0158 0.060 Uiso 1 1 calc R . .
H20B H 0.6225 0.8421 1.0907 0.060 Uiso 1 1 calc R . .
H20C H 0.6448 0.7905 0.9927 0.060 Uiso 1 1 calc R . .
C21B C 0.6975(3) 1.1018(2) 0.7803(2) 0.0399(7) Uani 1 1 d . . .
H21A H 0.6416 1.1529 0.7889 0.060 Uiso 1 1 calc R . .
H21B H 0.6813 1.0516 0.7384 0.060 Uiso 1 1 calc R . .
H21C H 0.7587 1.1312 0.7548 0.060 Uiso 1 1 calc R . .
C22B C 0.8300(3) 1.1258(2) 1.0838(2) 0.0412(8) Uani 1 1 d . . .
H22A H 0.8964 1.0914 1.0876 0.062 Uiso 1 1 calc R . .
H22B H 0.7920 1.1290 1.1445 0.062 Uiso 1 1 calc R . .
H22D H 0.8380 1.1926 1.0609 0.062 Uiso 1 1 calc R . .
B1 B 0.7133(2) 0.2432(2) 0.4614(2) 0.0208(6) Uani 1 1 d . . .
C11C C 0.70375(19) 0.13569(18) 0.41417(17) 0.0209(5) Uani 1 1 d . . .
C12C C 0.6242(2) 0.07691(19) 0.43526(18) 0.0243(6) Uani 1 1 d . . .
H12C H 0.5691 0.1018 0.4769 0.029 Uiso 1 1 calc R . .
C13C C 0.6212(2) -0.0163(2) 0.3986(2) 0.0310(6) Uani 1 1 d . . .
H13C H 0.5651 -0.0533 0.4155 0.037 Uiso 1 1 calc R . .
C14C C 0.6996(2) -0.0552(2) 0.33781(19) 0.0305(6) Uani 1 1 d . . .
H14C H 0.6990 -0.1195 0.3138 0.037 Uiso 1 1 calc R . .
C15C C 0.7789(2) 0.0009(2) 0.31251(19) 0.0307(6) Uani 1 1 d . . .
H15C H 0.8330 -0.0243 0.2699 0.037 Uiso 1 1 calc R . .
C16C C 0.7798(2) 0.09468(19) 0.34927(19) 0.0272(6) Uani 1 1 d . . .
H16C H 0.8345 0.1325 0.3295 0.033 Uiso 1 1 calc R . .
C21C C 0.73341(18) 0.32759(18) 0.38207(18) 0.0218(5) Uani 1 1 d . . .
C22C C 0.70506(18) 0.3195(2) 0.29403(18) 0.0249(6) Uani 1 1 d . . .
H22C H 0.6753 0.2618 0.2789 0.030 Uiso 1 1 calc R . .
C23C C 0.7182(2) 0.3914(2) 0.2277(2) 0.0310(6) Uani 1 1 d . . .
H23C H 0.6972 0.3823 0.1690 0.037 Uiso 1 1 calc R . .
C24C C 0.7617(2) 0.4761(2) 0.2470(2) 0.0328(7) Uani 1 1 d . . .
H24C H 0.7710 0.5256 0.2020 0.039 Uiso 1 1 calc R . .
C25C C 0.7913(2) 0.4875(2) 0.3325(2) 0.0328(7) Uani 1 1 d . . .
H25C H 0.8215 0.5453 0.3467 0.039 Uiso 1 1 calc R . .
C26C C 0.7772(2) 0.41507(19) 0.3983(2) 0.0280(6) Uani 1 1 d . . .
H26C H 0.7980 0.4251 0.4569 0.034 Uiso 1 1 calc R . .
C31C C 0.80671(19) 0.23718(19) 0.52627(18) 0.0249(6) Uani 1 1 d . . .
C32C C 0.8892(2) 0.1667(2) 0.5181(2) 0.0320(7) Uani 1 1 d . . .
H32C H 0.8931 0.1175 0.4723 0.038 Uiso 1 1 calc R . .
C33C C 0.9658(2) 0.1664(3) 0.5748(2) 0.0460(9) Uani 1 1 d . . .
H33C H 1.0199 0.1167 0.5679 0.055 Uiso 1 1 calc R . .
C34C C 0.9637(3) 0.2383(3) 0.6416(2) 0.0522(10) Uani 1 1 d . . .
H34C H 1.0159 0.2382 0.6802 0.063 Uiso 1 1 calc R . .
C35C C 0.8849(3) 0.3094(3) 0.6507(2) 0.0462(9) Uani 1 1 d . . .
H35C H 0.8826 0.3596 0.6954 0.055 Uiso 1 1 calc R . .
C36C C 0.8087(2) 0.3076(2) 0.59460(19) 0.0332(7) Uani 1 1 d . . .
H36C H 0.7545 0.3571 0.6029 0.040 Uiso 1 1 calc R . .
C41C C 0.60839(18) 0.27508(17) 0.52696(17) 0.0195(5) Uani 1 1 d . . .
C42C C 0.54023(19) 0.35498(18) 0.51098(18) 0.0233(6) Uani 1 1 d . . .
H42C H 0.5567 0.3973 0.4611 0.028 Uiso 1 1 calc R . .
C43C C 0.4489(2) 0.3748(2) 0.5656(2) 0.0277(6) Uani 1 1 d . . .
H43C H 0.4045 0.4295 0.5521 0.033 Uiso 1 1 calc R . .
C44C C 0.4229(2) 0.3153(2) 0.6392(2) 0.0290(6) Uani 1 1 d . . .
H44C H 0.3606 0.3280 0.6759 0.035 Uiso 1 1 calc R . .
C45C C 0.4895(2) 0.23640(19) 0.65844(18) 0.0255(6) Uani 1 1 d . . .
H45C H 0.4731 0.1951 0.7091 0.031 Uiso 1 1 calc R . .
C46C C 0.57973(19) 0.21805(18) 0.60367(17) 0.0221(5) Uani 1 1 d . . .
H46C H 0.6244 0.1643 0.6187 0.027 Uiso 1 1 calc R . .
C1D C 0.8832(3) 0.4846(3) 0.9194(3) 0.0619(11) Uani 1 1 d . . .
H1D1 H 0.8224 0.4911 0.8866 0.074 Uiso 1 1 calc R . .
H1D2 H 0.8926 0.5500 0.9442 0.074 Uiso 1 1 calc R . .
Cl1D Cl 0.98670(9) 0.44749(9) 0.84303(7) 0.0714(3) Uani 1 1 d . . .
Cl2D Cl 0.86467(9) 0.40275(11) 1.00912(8) 0.0831(4) Uani 1 1 d . . .
C1E C 0.1046(3) 0.2194(3) 0.9153(2) 0.0492(9) Uani 1 1 d . . .
H1E1 H 0.1439 0.1913 0.9637 0.059 Uiso 1 1 calc R . .
H1E2 H 0.0619 0.2773 0.9411 0.059 Uiso 1 1 calc R . .
Cl1E Cl 0.18741(8) 0.25648(7) 0.82290(8) 0.0655(3) Uani 1 1 d . . .
Cl2E Cl 0.02786(7) 0.13158(8) 0.88094(7) 0.0622(3) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Rh1 0.01323(10) 0.01653(10) 0.02008(11) -0.00243(7) -0.00153(7) -0.00226(7)
Cl1 0.0247(3) 0.0335(3) 0.0218(3) -0.0026(3) -0.0044(3) 0.0015(3)
C1A 0.0133(12) 0.0246(13) 0.0282(14) -0.0023(11) 0.0052(10) -0.0032(10)
C2A 0.0187(13) 0.0251(13) 0.0267(14) -0.0051(11) 0.0067(11) -0.0042(11)
C3A 0.0211(13) 0.0295(14) 0.0209(13) 0.0001(11) 0.0036(11) -0.0056(11)
C4A 0.0220(13) 0.0258(13) 0.0250(14) 0.0025(11) 0.0031(11) -0.0059(11)
C5A 0.0170(12) 0.0225(13) 0.0283(14) -0.0003(11) 0.0023(11) -0.0044(10)
C6A 0.0160(13) 0.0320(15) 0.0406(17) -0.0019(13) -0.0019(12) -0.0014(11)
C7A 0.0312(16) 0.0277(15) 0.0419(18) -0.0102(13) 0.0027(13) -0.0008(12)
C8A 0.0326(16) 0.0449(17) 0.0234(15) -0.0051(13) -0.0001(12) -0.0085(13)
C9A 0.0390(17) 0.0297(15) 0.0334(16) 0.0077(13) -0.0040(13) -0.0024(13)
C10A 0.0232(14) 0.0234(14) 0.0484(18) -0.0058(13) -0.0056(13) -0.0070(11)
N1B 0.0166(10) 0.0185(10) 0.0194(11) -0.0019(8) -0.0013(8) -0.0021(8)
N2B 0.0183(11) 0.0190(10) 0.0250(11) -0.0024(9) -0.0008(9) -0.0033(9)
N3B 0.0220(11) 0.0205(11) 0.0222(11) -0.0034(9) -0.0024(9) -0.0063(9)
N4B 0.0160(11) 0.0212(11) 0.0284(12) -0.0047(9) -0.0053(9) 0.0011(9)
N5B 0.0184(11) 0.0281(12) 0.0396(14) -0.0153(11) -0.0061(10) 0.0029(9)
C1B 0.0197(13) 0.0254(13) 0.0243(14) -0.0028(11) -0.0043(11) -0.0063(11)
C2B 0.0194(13) 0.0229(13) 0.0172(12) -0.0036(10) -0.0022(10) -0.0044(10)
C3B 0.0201(13) 0.0226(13) 0.0253(14) -0.0021(11) -0.0067(11) -0.0027(10)
C4B 0.0169(14) 0.0361(16) 0.0490(19) -0.0133(14) -0.0080(13) 0.0061(12)
C5B 0.0196(14) 0.0429(18) 0.060(2) -0.0263(16) -0.0068(14) 0.0105(13)
C6B 0.0196(13) 0.0186(12) 0.0236(13) -0.0025(10) -0.0025(10) -0.0028(10)
C7B 0.0306(15) 0.0167(12) 0.0325(15) -0.0031(11) -0.0025(12) -0.0048(11)
C8B 0.0324(15) 0.0138(12) 0.0315(15) -0.0035(11) -0.0013(12) -0.0072(11)
C9B 0.052(2) 0.0375(17) 0.0421(19) 0.0026(14) -0.0140(16) -0.0130(15)
C10B 0.106(4) 0.059(2) 0.035(2) 0.0070(17) -0.024(2) -0.038(2)
C11B 0.114(4) 0.046(2) 0.040(2) -0.0140(18) 0.024(2) -0.043(2)
C12B 0.060(2) 0.0297(17) 0.079(3) -0.0068(18) 0.036(2) -0.0119(17)
C13B 0.0380(18) 0.0284(15) 0.057(2) 0.0092(15) 0.0063(16) -0.0043(13)
C14B 0.0190(13) 0.0239(13) 0.0319(15) -0.0141(11) -0.0035(11) 0.0028(11)
C15B 0.0266(14) 0.0262(14) 0.0286(15) -0.0064(11) -0.0064(12) 0.0051(11)
C16B 0.0323(15) 0.0216(13) 0.0310(15) -0.0033(11) -0.0047(12) -0.0032(11)
C17B 0.0317(15) 0.0237(13) 0.0303(15) -0.0078(11) -0.0064(12) -0.0015(12)
C18B 0.0307(15) 0.0260(14) 0.0270(15) -0.0046(11) -0.0003(12) 0.0003(12)
C19B 0.0216(14) 0.0221(13) 0.0360(16) -0.0091(12) 0.0042(12) 0.0020(11)
C20B 0.0375(17) 0.0301(15) 0.0487(19) -0.0146(14) 0.0149(15) -0.0078(13)
C21B 0.053(2) 0.0341(16) 0.0339(17) -0.0032(13) -0.0171(15) 0.0067(15)
C22B 0.056(2) 0.0387(17) 0.0330(17) -0.0049(14) -0.0142(15) -0.0150(15)
B1 0.0191(14) 0.0209(14) 0.0224(15) 0.0003(12) -0.0005(12) -0.0039(12)
C11C 0.0205(13) 0.0205(12) 0.0214(13) 0.0029(10) -0.0019(10) -0.0014(10)
C12C 0.0220(13) 0.0269(14) 0.0236(14) -0.0039(11) -0.0003(11) -0.0022(11)
C13C 0.0301(15) 0.0306(15) 0.0330(16) -0.0027(12) 0.0009(13) -0.0124(12)
C14C 0.0387(17) 0.0226(13) 0.0304(15) -0.0057(12) -0.0024(13) -0.0042(12)
C15C 0.0322(15) 0.0295(14) 0.0277(15) -0.0051(12) 0.0064(12) 0.0005(12)
C16C 0.0263(14) 0.0243(13) 0.0299(15) -0.0009(11) 0.0043(12) -0.0056(11)
C21C 0.0149(12) 0.0225(13) 0.0263(14) -0.0005(11) 0.0041(10) 0.0010(10)
C22C 0.0153(12) 0.0288(14) 0.0307(15) 0.0045(12) -0.0016(11) -0.0044(11)
C23C 0.0209(14) 0.0422(17) 0.0298(15) 0.0084(13) -0.0035(12) -0.0011(12)
C24C 0.0252(15) 0.0299(15) 0.0399(17) 0.0143(13) 0.0070(13) 0.0025(12)
C25C 0.0300(15) 0.0226(14) 0.0434(18) 0.0013(12) 0.0073(13) -0.0035(12)
C26C 0.0290(15) 0.0248(14) 0.0296(15) -0.0039(11) 0.0017(12) -0.0039(12)
C31C 0.0198(13) 0.0294(14) 0.0257(14) 0.0070(11) 0.0008(11) -0.0073(11)
C32C 0.0220(14) 0.0351(16) 0.0390(17) 0.0096(13) -0.0025(12) -0.0054(12)
C33C 0.0219(15) 0.059(2) 0.057(2) 0.0241(18) -0.0047(15) -0.0036(15)
C34C 0.0337(19) 0.085(3) 0.044(2) 0.018(2) -0.0176(16) -0.0229(19)
C35C 0.0406(19) 0.072(2) 0.0299(17) -0.0019(16) -0.0091(14) -0.0207(18)
C36C 0.0268(15) 0.0446(17) 0.0289(15) -0.0042(13) -0.0025(12) -0.0068(13)
C41C 0.0190(13) 0.0184(12) 0.0221(13) -0.0060(10) -0.0033(10) -0.0061(10)
C42C 0.0252(14) 0.0203(13) 0.0251(14) -0.0011(11) -0.0040(11) -0.0055(11)
C43C 0.0202(13) 0.0246(13) 0.0388(16) -0.0065(12) -0.0062(12) -0.0006(11)
C44C 0.0189(13) 0.0341(15) 0.0337(16) -0.0115(13) 0.0031(12) -0.0073(12)
C45C 0.0282(14) 0.0260(13) 0.0230(14) -0.0043(11) 0.0013(11) -0.0117(11)
C46C 0.0233(13) 0.0207(12) 0.0230(13) -0.0038(10) -0.0043(11) -0.0034(10)
C1D 0.053(2) 0.054(2) 0.076(3) 0.016(2) -0.005(2) 0.0110(19)
Cl1D 0.0709(7) 0.0830(7) 0.0565(6) 0.0126(5) 0.0034(5) 0.0018(6)
Cl2D 0.0598(7) 0.1232(10) 0.0646(7) 0.0320(7) 0.0013(5) -0.0112(7)
C1E 0.051(2) 0.051(2) 0.046(2) -0.0142(16) -0.0117(17) 0.0041(17)
Cl1E 0.0566(6) 0.0507(5) 0.0856(8) -0.0018(5) 0.0067(5) -0.0014(4)
Cl2E 0.0487(5) 0.0770(7) 0.0623(6) -0.0152(5) -0.0045(5) -0.0136(5)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 C6B 2.076(3) . ?
Rh1 N1B 2.1090(19) . ?
Rh1 C5A 2.147(2) . ?
Rh1 C3A 2.170(3) . ?
Rh1 C4A 2.175(2) . ?
Rh1 C2A 2.215(3) . ?
Rh1 C1A 2.215(2) . ?
Rh1 Cl1 2.3774(6) . ?
C1A C2A 1.410(4) . ?
C1A C5A 1.459(4) . ?
C1A C6A 1.490(4) . ?
C2A C3A 1.451(4) . ?
C2A C7A 1.495(4) . ?
C3A C4A 1.424(4) . ?
C3A C8A 1.499(4) . ?
C4A C5A 1.435(4) . ?
C4A C9A 1.497(4) . ?
C5A C10A 1.499(4) . ?
C6A H6A1 0.9800 . ?
C6A H6A2 0.9800 . ?
C6A H6A3 0.9800 . ?
C7A H7A1 0.9800 . ?
C7A H7A2 0.9800 . ?
C7A H7A3 0.9800 . ?
C8A H8A1 0.9800 . ?
C8A H8A2 0.9800 . ?
C8A H8A3 0.9800 . ?
C9A H9A1 0.9800 . ?
C9A H9A2 0.9800 . ?
C9A H9A3 0.9800 . ?
C10A H10A 0.9800 . ?
C10A H10C 0.9800 . ?
C10A H10D 0.9800 . ?
N1B N2B 1.320(3) . ?
N1B C2B 1.359(3) . ?
N2B N3B 1.338(3) . ?
N3B C1B 1.344(3) . ?
N3B C7B 1.479(3) . ?
N4B C6B 1.364(3) . ?
N4B C4B 1.383(4) . ?
N4B C3B 1.466(3) . ?
N5B C6B 1.359(3) . ?
N5B C5B 1.389(4) . ?
N5B C14B 1.450(3) . ?
C1B C2B 1.366(3) . ?
C1B H1B 0.9500 . ?
C2B C3B 1.493(3) . ?
C3B H3B1 0.9900 . ?
C3B H3B2 0.9900 . ?
C4B C5B 1.330(4) . ?
C4B H4B 0.9500 . ?
C5B H5B 0.9500 . ?
C7B C8B 1.508(4) . ?
C7B H7B1 0.9900 . ?
C7B H7B2 0.9900 . ?
C8B C13B 1.378(4) . ?
C8B C9B 1.382(4) . ?
C9B C10B 1.390(5) . ?
C9B H9B 0.9500 . ?
C10B C11B 1.361(6) . ?
C10B H10B 0.9500 . ?
C11B C12B 1.359(6) . ?
C11B H11B 0.9500 . ?
C12B C13B 1.380(5) . ?
C12B H12B 0.9500 . ?
C13B H13B 0.9500 . ?
C14B C19B 1.395(4) . ?
C14B C15B 1.395(4) . ?
C15B C16B 1.393(4) . ?
C15B C21B 1.506(4) . ?
C16B C17B 1.379(4) . ?
C16B H16B 0.9500 . ?
C17B C18B 1.392(4) . ?
C17B C22B 1.514(4) . ?
C18B C19B 1.390(4) . ?
C18B H18B 0.9500 . ?
C19B C20B 1.507(4) . ?
C20B H20A 0.9800 . ?
C20B H20B 0.9800 . ?
C20B H20C 0.9800 . ?
C21B H21A 0.9800 . ?
C21B H21B 0.9800 . ?
C21B H21C 0.9800 . ?
C22B H22A 0.9800 . ?
C22B H22B 0.9800 . ?
C22B H22D 0.9800 . ?
B1 C41C 1.648(4) . ?
B1 C11C 1.649(4) . ?
B1 C21C 1.653(4) . ?
B1 C31C 1.654(4) . ?
C11C C12C 1.394(4) . ?
C11C C16C 1.404(4) . ?
C12C C13C 1.392(4) . ?
C12C H12C 0.9500 . ?
C13C C14C 1.379(4) . ?
C13C H13C 0.9500 . ?
C14C C15C 1.378(4) . ?
C14C H14C 0.9500 . ?
C15C C16C 1.395(4) . ?
C15C H15C 0.9500 . ?
C16C H16C 0.9500 . ?
C21C C22C 1.400(4) . ?
C21C C26C 1.406(4) . ?
C22C C23C 1.389(4) . ?
C22C H22C 0.9500 . ?
C23C C24C 1.382(4) . ?
C23C H23C 0.9500 . ?
C24C C25C 1.376(4) . ?
C24C H24C 0.9500 . ?
C25C C26C 1.391(4) . ?
C25C H25C 0.9500 . ?
C26C H26C 0.9500 . ?
C31C C36C 1.401(4) . ?
C31C C32C 1.402(4) . ?
C32C C33C 1.395(4) . ?
C32C H32C 0.9500 . ?
C33C C34C 1.391(5) . ?
C33C H33C 0.9500 . ?
C34C C35C 1.371(5) . ?
C34C H34C 0.9500 . ?
C35C C36C 1.386(4) . ?
C35C H35C 0.9500 . ?
C36C H36C 0.9500 . ?
C41C C42C 1.401(4) . ?
C41C C46C 1.405(3) . ?
C42C C43C 1.399(4) . ?
C42C H42C 0.9500 . ?
C43C C44C 1.382(4) . ?
C43C H43C 0.9500 . ?
C44C C45C 1.391(4) . ?
C44C H44C 0.9500 . ?
C45C C46C 1.386(4) . ?
C45C H45C 0.9500 . ?
C46C H46C 0.9500 . ?
C1D Cl1D 1.733(4) . ?
C1D Cl2D 1.736(4) . ?
C1D H1D1 0.9900 . ?
C1D H1D2 0.9900 . ?
C1E Cl2E 1.754(4) . ?
C1E Cl1E 1.760(4) . ?
C1E H1E1 0.9900 . ?
C1E H1E2 0.9900 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6B Rh1 N1B 83.97(9) . . ?
C6B Rh1 C5A 110.94(10) . . ?
N1B Rh1 C5A 160.05(9) . . ?
C6B Rh1 C3A 118.39(10) . . ?
N1B Rh1 C3A 96.85(9) . . ?
C5A Rh1 C3A 64.73(10) . . ?
C6B Rh1 C4A 97.61(10) . . ?
N1B Rh1 C4A 128.98(9) . . ?
C5A Rh1 C4A 38.77(10) . . ?
C3A Rh1 C4A 38.25(10) . . ?
C6B Rh1 C2A 157.01(10) . . ?
N1B Rh1 C2A 96.65(9) . . ?
C5A Rh1 C2A 64.37(10) . . ?
C3A Rh1 C2A 38.63(10) . . ?
C4A Rh1 C2A 64.15(10) . . ?
C6B Rh1 C1A 148.73(10) . . ?
N1B Rh1 C1A 127.29(9) . . ?
C5A Rh1 C1A 39.04(9) . . ?
C3A Rh1 C1A 63.66(10) . . ?
C4A Rh1 C1A 64.21(10) . . ?
C2A Rh1 C1A 37.13(10) . . ?
C6B Rh1 Cl1 90.79(7) . . ?
N1B Rh1 Cl1 88.82(6) . . ?
C5A Rh1 Cl1 103.65(7) . . ?
C3A Rh1 Cl1 150.64(7) . . ?
C4A Rh1 Cl1 141.83(7) . . ?
C2A Rh1 Cl1 112.19(7) . . ?
C1A Rh1 Cl1 90.05(7) . . ?
C2A C1A C5A 108.2(2) . . ?
C2A C1A C6A 126.5(2) . . ?
C5A C1A C6A 125.4(2) . . ?
C2A C1A Rh1 71.43(14) . . ?
C5A C1A Rh1 67.97(13) . . ?
C6A C1A Rh1 125.69(18) . . ?
C1A C2A C3A 107.9(2) . . ?
C1A C2A C7A 127.0(3) . . ?
C3A C2A C7A 125.1(2) . . ?
C1A C2A Rh1 71.45(14) . . ?
C3A C2A Rh1 69.02(14) . . ?
C7A C2A Rh1 127.87(18) . . ?
C4A C3A C2A 108.4(2) . . ?
C4A C3A C8A 126.7(2) . . ?
C2A C3A C8A 124.3(2) . . ?
C4A C3A Rh1 71.04(15) . . ?
C2A C3A Rh1 72.35(14) . . ?
C8A C3A Rh1 129.27(18) . . ?
C3A C4A C5A 107.9(2) . . ?
C3A C4A C9A 124.3(2) . . ?
C5A C4A C9A 127.7(2) . . ?
C3A C4A Rh1 70.70(14) . . ?
C5A C4A Rh1 69.58(14) . . ?
C9A C4A Rh1 128.23(19) . . ?
C4A C5A C1A 107.5(2) . . ?
C4A C5A C10A 127.5(2) . . ?
C1A C5A C10A 124.3(2) . . ?
C4A C5A Rh1 71.65(14) . . ?
C1A C5A Rh1 72.99(14) . . ?
C10A C5A Rh1 128.42(19) . . ?
C1A C6A H6A1 109.5 . . ?
C1A C6A H6A2 109.5 . . ?
H6A1 C6A H6A2 109.5 . . ?
C1A C6A H6A3 109.5 . . ?
H6A1 C6A H6A3 109.5 . . ?
H6A2 C6A H6A3 109.5 . . ?
C2A C7A H7A1 109.5 . . ?
C2A C7A H7A2 109.5 . . ?
H7A1 C7A H7A2 109.5 . . ?
C2A C7A H7A3 109.5 . . ?
H7A1 C7A H7A3 109.5 . . ?
H7A2 C7A H7A3 109.5 . . ?
C3A C8A H8A1 109.5 . . ?
C3A C8A H8A2 109.5 . . ?
H8A1 C8A H8A2 109.5 . . ?
C3A C8A H8A3 109.5 . . ?
H8A1 C8A H8A3 109.5 . . ?
H8A2 C8A H8A3 109.5 . . ?
C4A C9A H9A1 109.5 . . ?
C4A C9A H9A2 109.5 . . ?
H9A1 C9A H9A2 109.5 . . ?
C4A C9A H9A3 109.5 . . ?
H9A1 C9A H9A3 109.5 . . ?
H9A2 C9A H9A3 109.5 . . ?
C5A C10A H10A 109.5 . . ?
C5A C10A H10C 109.5 . . ?
H10A C10A H10C 109.5 . . ?
C5A C10A H10D 109.5 . . ?
H10A C10A H10D 109.5 . . ?
H10C C10A H10D 109.5 . . ?
N2B N1B C2B 110.57(19) . . ?
N2B N1B Rh1 126.79(15) . . ?
C2B N1B Rh1 122.61(16) . . ?
N1B N2B N3B 105.31(19) . . ?
N2B N3B C1B 112.1(2) . . ?
N2B N3B C7B 119.9(2) . . ?
C1B N3B C7B 128.0(2) . . ?
C6B N4B C4B 111.6(2) . . ?
C6B N4B C3B 124.0(2) . . ?
C4B N4B C3B 124.3(2) . . ?
C6B N5B C5B 110.4(2) . . ?
C6B N5B C14B 129.8(2) . . ?
C5B N5B C14B 119.7(2) . . ?
N3B C1B C2B 105.0(2) . . ?
N3B C1B H1B 127.5 . . ?
C2B C1B H1B 127.5 . . ?
N1B C2B C1B 107.1(2) . . ?
N1B C2B C3B 119.6(2) . . ?
C1B C2B C3B 133.3(2) . . ?
N4B C3B C2B 109.8(2) . . ?
N4B C3B H3B1 109.7 . . ?
C2B C3B H3B1 109.7 . . ?
N4B C3B H3B2 109.7 . . ?
C2B C3B H3B2 109.7 . . ?
H3B1 C3B H3B2 108.2 . . ?
C5B C4B N4B 106.2(2) . . ?
C5B C4B H4B 126.9 . . ?
N4B C4B H4B 126.9 . . ?
C4B C5B N5B 107.9(3) . . ?
C4B C5B H5B 126.1 . . ?
N5B C5B H5B 126.1 . . ?
N5B C6B N4B 103.8(2) . . ?
N5B C6B Rh1 136.22(18) . . ?
N4B C6B Rh1 119.79(18) . . ?
N3B C7B C8B 112.6(2) . . ?
N3B C7B H7B1 109.1 . . ?
C8B C7B H7B1 109.1 . . ?
N3B C7B H7B2 109.1 . . ?
C8B C7B H7B2 109.1 . . ?
H7B1 C7B H7B2 107.8 . . ?
C13B C8B C9B 118.6(3) . . ?
C13B C8B C7B 121.4(3) . . ?
C9B C8B C7B 119.9(3) . . ?
C8B C9B C10B 119.8(4) . . ?
C8B C9B H9B 120.1 . . ?
C10B C9B H9B 120.1 . . ?
C11B C10B C9B 120.3(4) . . ?
C11B C10B H10B 119.8 . . ?
C9B C10B H10B 119.8 . . ?
C12B C11B C10B 120.4(4) . . ?
C12B C11B H11B 119.8 . . ?
C10B C11B H11B 119.8 . . ?
C11B C12B C13B 119.8(4) . . ?
C11B C12B H12B 120.1 . . ?
C13B C12B H12B 120.1 . . ?
C8B C13B C12B 120.9(3) . . ?
C8B C13B H13B 119.5 . . ?
C12B C13B H13B 119.5 . . ?
C19B C14B C15B 121.7(2) . . ?
C19B C14B N5B 118.8(2) . . ?
C15B C14B N5B 118.8(2) . . ?
C16B C15B C14B 117.8(3) . . ?
C16B C15B C21B 119.5(3) . . ?
C14B C15B C21B 122.6(3) . . ?
C17B C16B C15B 122.1(3) . . ?
C17B C16B H16B 118.9 . . ?
C15B C16B H16B 118.9 . . ?
C16B C17B C18B 118.3(3) . . ?
C16B C17B C22B 120.8(3) . . ?
C18B C17B C22B 120.9(3) . . ?
C19B C18B C17B 121.9(3) . . ?
C19B C18B H18B 119.1 . . ?
C17B C18B H18B 119.1 . . ?
C18B C19B C14B 117.9(2) . . ?
C18B C19B C20B 120.3(3) . . ?
C14B C19B C20B 121.7(3) . . ?
C19B C20B H20A 109.5 . . ?
C19B C20B H20B 109.5 . . ?
H20A C20B H20B 109.5 . . ?
C19B C20B H20C 109.5 . . ?
H20A C20B H20C 109.5 . . ?
H20B C20B H20C 109.5 . . ?
C15B C21B H21A 109.5 . . ?
C15B C21B H21B 109.5 . . ?
H21A C21B H21B 109.5 . . ?
C15B C21B H21C 109.5 . . ?
H21A C21B H21C 109.5 . . ?
H21B C21B H21C 109.5 . . ?
C17B C22B H22A 109.5 . . ?
C17B C22B H22B 109.5 . . ?
H22A C22B H22B 109.5 . . ?
C17B C22B H22D 109.5 . . ?
H22A C22B H22D 109.5 . . ?
H22B C22B H22D 109.5 . . ?
C41C B1 C11C 109.0(2) . . ?
C41C B1 C21C 109.7(2) . . ?
C11C B1 C21C 110.5(2) . . ?
C41C B1 C31C 107.8(2) . . ?
C11C B1 C31C 110.9(2) . . ?
C21C B1 C31C 108.9(2) . . ?
C12C C11C C16C 114.3(2) . . ?
C12C C11C B1 124.8(2) . . ?
C16C C11C B1 120.9(2) . . ?
C13C C12C C11C 123.5(3) . . ?
C13C C12C H12C 118.2 . . ?
C11C C12C H12C 118.2 . . ?
C14C C13C C12C 120.1(3) . . ?
C14C C13C H13C 120.0 . . ?
C12C C13C H13C 120.0 . . ?
C15C C14C C13C 118.8(3) . . ?
C15C C14C H14C 120.6 . . ?
C13C C14C H14C 120.6 . . ?
C14C C15C C16C 120.1(3) . . ?
C14C C15C H15C 119.9 . . ?
C16C C15C H15C 119.9 . . ?
C15C C16C C11C 123.0(2) . . ?
C15C C16C H16C 118.5 . . ?
C11C C16C H16C 118.5 . . ?
C22C C21C C26C 114.4(2) . . ?
C22C C21C B1 122.7(2) . . ?
C26C C21C B1 122.8(2) . . ?
C23C C22C C21C 123.4(3) . . ?
C23C C22C H22C 118.3 . . ?
C21C C22C H22C 118.3 . . ?
C24C C23C C22C 120.0(3) . . ?
C24C C23C H23C 120.0 . . ?
C22C C23C H23C 120.0 . . ?
C25C C24C C23C 118.9(3) . . ?
C25C C24C H24C 120.5 . . ?
C23C C24C H24C 120.5 . . ?
C24C C25C C26C 120.4(3) . . ?
C24C C25C H25C 119.8 . . ?
C26C C25C H25C 119.8 . . ?
C25C C26C C21C 122.9(3) . . ?
C25C C26C H26C 118.5 . . ?
C21C C26C H26C 118.5 . . ?
C36C C31C C32C 114.7(3) . . ?
C36C C31C B1 120.1(2) . . ?
C32C C31C B1 125.2(3) . . ?
C33C C32C C31C 122.2(3) . . ?
C33C C32C H32C 118.9 . . ?
C31C C32C H32C 118.9 . . ?
C34C C33C C32C 120.5(3) . . ?
C34C C33C H33C 119.7 . . ?
C32C C33C H33C 119.7 . . ?
C35C C34C C33C 119.0(3) . . ?
C35C C34C H34C 120.5 . . ?
C33C C34C H34C 120.5 . . ?
C34C C35C C36C 119.7(3) . . ?
C34C C35C H35C 120.2 . . ?
C36C C35C H35C 120.2 . . ?
C35C C36C C31C 124.0(3) . . ?
C35C C36C H36C 118.0 . . ?
C31C C36C H36C 118.0 . . ?
C42C C41C C46C 115.1(2) . . ?
C42C C41C B1 125.0(2) . . ?
C46C C41C B1 119.9(2) . . ?
C43C C42C C41C 122.5(2) . . ?
C43C C42C H42C 118.7 . . ?
C41C C42C H42C 118.7 . . ?
C44C C43C C42C 120.3(2) . . ?
C44C C43C H43C 119.9 . . ?
C42C C43C H43C 119.9 . . ?
C43C C44C C45C 118.9(3) . . ?
C43C C44C H44C 120.5 . . ?
C45C C44C H44C 120.5 . . ?
C46C C45C C44C 119.9(2) . . ?
C46C C45C H45C 120.0 . . ?
C44C C45C H45C 120.0 . . ?
C45C C46C C41C 123.2(2) . . ?
C45C C46C H46C 118.4 . . ?
C41C C46C H46C 118.4 . . ?
Cl1D C1D Cl2D 112.4(2) . . ?
Cl1D C1D H1D1 109.1 . . ?
Cl2D C1D H1D1 109.1 . . ?
Cl1D C1D H1D2 109.1 . . ?
Cl2D C1D H1D2 109.1 . . ?
H1D1 C1D H1D2 107.8 . . ?
Cl2E C1E Cl1E 111.06(19) . . ?
Cl2E C1E H1E1 109.4 . . ?
Cl1E C1E H1E1 109.4 . . ?
Cl2E C1E H1E2 109.4 . . ?
Cl1E C1E H1E2 109.4 . . ?
H1E1 C1E H1E2 108.0 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6B Rh1 C1A C2A -139.74(19) . . . . ?
N1B Rh1 C1A C2A 40.10(19) . . . . ?
C5A Rh1 C1A C2A -119.4(2) . . . . ?
C3A Rh1 C1A C2A -37.79(15) . . . . ?
C4A Rh1 C1A C2A -80.57(17) . . . . ?
Cl1 Rh1 C1A C2A 128.65(14) . . . . ?
C6B Rh1 C1A C5A -20.3(3) . . . . ?
N1B Rh1 C1A C5A 159.51(14) . . . . ?
C3A Rh1 C1A C5A 81.62(16) . . . . ?
C4A Rh1 C1A C5A 38.84(15) . . . . ?
C2A Rh1 C1A C5A 119.4(2) . . . . ?
Cl1 Rh1 C1A C5A -111.94(14) . . . . ?
C6B Rh1 C1A C6A 98.2(3) . . . . ?
N1B Rh1 C1A C6A -81.9(2) . . . . ?
C5A Rh1 C1A C6A 118.6(3) . . . . ?
C3A Rh1 C1A C6A -159.8(3) . . . . ?
C4A Rh1 C1A C6A 157.4(3) . . . . ?
C2A Rh1 C1A C6A -122.0(3) . . . . ?
Cl1 Rh1 C1A C6A 6.6(2) . . . . ?
C5A C1A C2A C3A 1.5(3) . . . . ?
C6A C1A C2A C3A -179.2(2) . . . . ?
Rh1 C1A C2A C3A 59.65(17) . . . . ?
C5A C1A C2A C7A 177.9(2) . . . . ?
C6A C1A C2A C7A -2.8(4) . . . . ?
Rh1 C1A C2A C7A -123.9(3) . . . . ?
C5A C1A C2A Rh1 -58.20(17) . . . . ?
C6A C1A C2A Rh1 121.1(3) . . . . ?
C6B Rh1 C2A C1A 120.8(2) . . . . ?
N1B Rh1 C2A C1A -148.94(15) . . . . ?
C5A Rh1 C2A C1A 37.49(15) . . . . ?
C3A Rh1 C2A C1A 118.4(2) . . . . ?
C4A Rh1 C2A C1A 80.73(16) . . . . ?
Cl1 Rh1 C2A C1A -57.50(15) . . . . ?
C6B Rh1 C2A C3A 2.4(3) . . . . ?
N1B Rh1 C2A C3A 92.66(14) . . . . ?
C5A Rh1 C2A C3A -80.91(16) . . . . ?
C4A Rh1 C2A C3A -37.67(15) . . . . ?
C1A Rh1 C2A C3A -118.4(2) . . . . ?
Cl1 Rh1 C2A C3A -175.90(12) . . . . ?
C6B Rh1 C2A C7A -116.3(3) . . . . ?
N1B Rh1 C2A C7A -26.1(3) . . . . ?
C5A Rh1 C2A C7A 160.3(3) . . . . ?
C3A Rh1 C2A C7A -118.8(3) . . . . ?
C4A Rh1 C2A C7A -156.4(3) . . . . ?
C1A Rh1 C2A C7A 122.8(3) . . . . ?
Cl1 Rh1 C2A C7A 65.3(3) . . . . ?
C1A C2A C3A C4A 1.1(3) . . . . ?
C7A C2A C3A C4A -175.4(2) . . . . ?
Rh1 C2A C3A C4A 62.29(17) . . . . ?
C1A C2A C3A C8A 172.9(2) . . . . ?
C7A C2A C3A C8A -3.7(4) . . . . ?
Rh1 C2A C3A C8A -126.0(3) . . . . ?
C1A C2A C3A Rh1 -61.19(17) . . . . ?
C7A C2A C3A Rh1 122.3(3) . . . . ?
C6B Rh1 C3A C4A 63.73(17) . . . . ?
N1B Rh1 C3A C4A 150.56(15) . . . . ?
C5A Rh1 C3A C4A -37.45(15) . . . . ?
C2A Rh1 C3A C4A -117.3(2) . . . . ?
C1A Rh1 C3A C4A -81.01(16) . . . . ?
Cl1 Rh1 C3A C4A -109.58(17) . . . . ?
C6B Rh1 C3A C2A -178.93(14) . . . . ?
N1B Rh1 C3A C2A -92.10(14) . . . . ?
C5A Rh1 C3A C2A 79.89(15) . . . . ?
C4A Rh1 C3A C2A 117.3(2) . . . . ?
C1A Rh1 C3A C2A 36.33(14) . . . . ?
Cl1 Rh1 C3A C2A 7.8(2) . . . . ?
C6B Rh1 C3A C8A -58.7(3) . . . . ?
N1B Rh1 C3A C8A 28.1(3) . . . . ?
C5A Rh1 C3A C8A -159.9(3) . . . . ?
C4A Rh1 C3A C8A -122.4(3) . . . . ?
C2A Rh1 C3A C8A 120.2(3) . . . . ?
C1A Rh1 C3A C8A 156.6(3) . . . . ?
Cl1 Rh1 C3A C8A 128.0(2) . . . . ?
C2A C3A C4A C5A -3.2(3) . . . . ?
C8A C3A C4A C5A -174.7(2) . . . . ?
Rh1 C3A C4A C5A 59.88(17) . . . . ?
C2A C3A C4A C9A 173.2(2) . . . . ?
C8A C3A C4A C9A 1.7(4) . . . . ?
Rh1 C3A C4A C9A -123.7(3) . . . . ?
C2A C3A C4A Rh1 -63.13(17) . . . . ?
C8A C3A C4A Rh1 125.4(3) . . . . ?
C6B Rh1 C4A C3A -127.26(16) . . . . ?
N1B Rh1 C4A C3A -38.88(19) . . . . ?
C5A Rh1 C4A C3A 118.6(2) . . . . ?
C2A Rh1 C4A C3A 38.04(15) . . . . ?
C1A Rh1 C4A C3A 79.46(16) . . . . ?
Cl1 Rh1 C4A C3A 131.64(14) . . . . ?
C6B Rh1 C4A C5A 114.17(16) . . . . ?
N1B Rh1 C4A C5A -157.45(14) . . . . ?
C3A Rh1 C4A C5A -118.6(2) . . . . ?
C2A Rh1 C4A C5A -80.53(16) . . . . ?
C1A Rh1 C4A C5A -39.11(15) . . . . ?
Cl1 Rh1 C4A C5A 13.1(2) . . . . ?
C6B Rh1 C4A C9A -8.3(3) . . . . ?
N1B Rh1 C4A C9A 80.1(3) . . . . ?
C5A Rh1 C4A C9A -122.5(3) . . . . ?
C3A Rh1 C4A C9A 119.0(3) . . . . ?
C2A Rh1 C4A C9A 157.0(3) . . . . ?
C1A Rh1 C4A C9A -161.6(3) . . . . ?
Cl1 Rh1 C4A C9A -109.4(2) . . . . ?
C3A C4A C5A C1A 4.1(3) . . . . ?
C9A C4A C5A C1A -172.2(3) . . . . ?
Rh1 C4A C5A C1A 64.69(17) . . . . ?
C3A C4A C5A C10A 174.6(2) . . . . ?
C9A C4A C5A C10A -1.6(4) . . . . ?
Rh1 C4A C5A C10A -124.8(3) . . . . ?
C3A C4A C5A Rh1 -60.59(17) . . . . ?
C9A C4A C5A Rh1 123.1(3) . . . . ?
C2A C1A C5A C4A -3.4(3) . . . . ?
C6A C1A C5A C4A 177.2(2) . . . . ?
Rh1 C1A C5A C4A -63.80(17) . . . . ?
C2A C1A C5A C10A -174.3(2) . . . . ?
C6A C1A C5A C10A 6.3(4) . . . . ?
Rh1 C1A C5A C10A 125.3(3) . . . . ?
C2A C1A C5A Rh1 60.36(17) . . . . ?
C6A C1A C5A Rh1 -119.0(2) . . . . ?
C6B Rh1 C5A C4A -75.52(17) . . . . ?
N1B Rh1 C5A C4A 60.9(3) . . . . ?
C3A Rh1 C5A C4A 36.96(15) . . . . ?
C2A Rh1 C5A C4A 79.93(17) . . . . ?
C1A Rh1 C5A C4A 115.6(2) . . . . ?
Cl1 Rh1 C5A C4A -171.73(14) . . . . ?
C6B Rh1 C5A C1A 168.87(15) . . . . ?
N1B Rh1 C5A C1A -54.7(3) . . . . ?
C3A Rh1 C5A C1A -78.65(16) . . . . ?
C4A Rh1 C5A C1A -115.6(2) . . . . ?
C2A Rh1 C5A C1A -35.67(15) . . . . ?
Cl1 Rh1 C5A C1A 72.66(15) . . . . ?
C6B Rh1 C5A C10A 48.2(3) . . . . ?
N1B Rh1 C5A C10A -175.4(2) . . . . ?
C3A Rh1 C5A C10A 160.7(3) . . . . ?
C4A Rh1 C5A C10A 123.7(3) . . . . ?
C2A Rh1 C5A C10A -156.4(3) . . . . ?
C1A Rh1 C5A C10A -120.7(3) . . . . ?
Cl1 Rh1 C5A C10A -48.0(2) . . . . ?
C6B Rh1 N1B N2B -140.8(2) . . . . ?
C5A Rh1 N1B N2B 79.5(3) . . . . ?
C3A Rh1 N1B N2B 101.2(2) . . . . ?
C4A Rh1 N1B N2B 124.3(2) . . . . ?
C2A Rh1 N1B N2B 62.3(2) . . . . ?
C1A Rh1 N1B N2B 39.3(2) . . . . ?
Cl1 Rh1 N1B N2B -49.90(19) . . . . ?
C6B Rh1 N1B C2B 41.45(19) . . . . ?
C5A Rh1 N1B C2B -98.2(3) . . . . ?
C3A Rh1 N1B C2B -76.5(2) . . . . ?
C4A Rh1 N1B C2B -53.5(2) . . . . ?
C2A Rh1 N1B C2B -115.4(2) . . . . ?
C1A Rh1 N1B C2B -138.47(19) . . . . ?
Cl1 Rh1 N1B C2B 132.37(19) . . . . ?
C2B N1B N2B N3B 0.1(3) . . . . ?
Rh1 N1B N2B N3B -177.86(15) . . . . ?
N1B N2B N3B C1B -0.3(3) . . . . ?
N1B N2B N3B C7B -178.6(2) . . . . ?
N2B N3B C1B C2B 0.4(3) . . . . ?
C7B N3B C1B C2B 178.6(2) . . . . ?
N2B N1B C2B C1B 0.1(3) . . . . ?
Rh1 N1B C2B C1B 178.19(17) . . . . ?
N2B N1B C2B C3B 178.9(2) . . . . ?
Rh1 N1B C2B C3B -3.0(3) . . . . ?
N3B C1B C2B N1B -0.3(3) . . . . ?
N3B C1B C2B C3B -178.9(3) . . . . ?
C6B N4B C3B C2B 55.2(3) . . . . ?
C4B N4B C3B C2B -121.2(3) . . . . ?
N1B C2B C3B N4B -51.6(3) . . . . ?
C1B C2B C3B N4B 126.9(3) . . . . ?
C6B N4B C4B C5B 0.2(3) . . . . ?
C3B N4B C4B C5B 177.0(3) . . . . ?
N4B C4B C5B N5B 0.0(4) . . . . ?
C6B N5B C5B C4B -0.2(4) . . . . ?
C14B N5B C5B C4B 177.9(3) . . . . ?
C5B N5B C6B N4B 0.3(3) . . . . ?
C14B N5B C6B N4B -177.6(3) . . . . ?
C5B N5B C6B Rh1 -175.1(2) . . . . ?
C14B N5B C6B Rh1 7.1(5) . . . . ?
C4B N4B C6B N5B -0.3(3) . . . . ?
C3B N4B C6B N5B -177.1(2) . . . . ?
C4B N4B C6B Rh1 176.02(19) . . . . ?
C3B N4B C6B Rh1 -0.8(3) . . . . ?
N1B Rh1 C6B N5B 136.0(3) . . . . ?
C5A Rh1 C6B N5B -57.7(3) . . . . ?
C3A Rh1 C6B N5B -129.5(3) . . . . ?
C4A Rh1 C6B N5B -95.4(3) . . . . ?
C2A Rh1 C6B N5B -131.2(3) . . . . ?
C1A Rh1 C6B N5B -44.2(4) . . . . ?
Cl1 Rh1 C6B N5B 47.2(3) . . . . ?
N1B Rh1 C6B N4B -38.85(19) . . . . ?
C5A Rh1 C6B N4B 127.47(19) . . . . ?
C3A Rh1 C6B N4B 55.7(2) . . . . ?
C4A Rh1 C6B N4B 89.8(2) . . . . ?
C2A Rh1 C6B N4B 54.0(3) . . . . ?
C1A Rh1 C6B N4B 141.0(2) . . . . ?
Cl1 Rh1 C6B N4B -127.58(19) . . . . ?
N2B N3B C7B C8B 92.6(3) . . . . ?
C1B N3B C7B C8B -85.5(3) . . . . ?
N3B C7B C8B C13B 66.9(3) . . . . ?
N3B C7B C8B C9B -114.3(3) . . . . ?
C13B C8B C9B C10B -0.1(4) . . . . ?
C7B C8B C9B C10B -179.0(3) . . . . ?
C8B C9B C10B C11B -1.3(5) . . . . ?
C9B C10B C11B C12B 1.4(6) . . . . ?
C10B C11B C12B C13B -0.2(5) . . . . ?
C9B C8B C13B C12B 1.4(4) . . . . ?
C7B C8B C13B C12B -179.8(3) . . . . ?
C11B C12B C13B C8B -1.2(5) . . . . ?
C6B N5B C14B C19B -99.0(3) . . . . ?
C5B N5B C14B C19B 83.3(3) . . . . ?
C6B N5B C14B C15B 90.3(3) . . . . ?
C5B N5B C14B C15B -87.4(3) . . . . ?
C19B C14B C15B C16B 7.4(4) . . . . ?
N5B C14B C15B C16B 177.8(2) . . . . ?
C19B C14B C15B C21B -167.9(3) . . . . ?
N5B C14B C15B C21B 2.5(4) . . . . ?
C14B C15B C16B C17B -3.4(4) . . . . ?
C21B C15B C16B C17B 172.1(3) . . . . ?
C15B C16B C17B C18B -1.1(4) . . . . ?
C15B C16B C17B C22B -179.5(3) . . . . ?
C16B C17B C18B C19B 1.8(4) . . . . ?
C22B C17B C18B C19B -179.8(3) . . . . ?
C17B C18B C19B C14B 2.0(4) . . . . ?
C17B C18B C19B C20B -175.4(3) . . . . ?
C15B C14B C19B C18B -6.7(4) . . . . ?
N5B C14B C19B C18B -177.1(2) . . . . ?
C15B C14B C19B C20B 170.6(3) . . . . ?
N5B C14B C19B C20B 0.2(4) . . . . ?
C41C B1 C11C C12C -6.9(3) . . . . ?
C21C B1 C11C C12C -127.5(3) . . . . ?
C31C B1 C11C C12C 111.7(3) . . . . ?
C41C B1 C11C C16C 175.0(2) . . . . ?
C21C B1 C11C C16C 54.3(3) . . . . ?
C31C B1 C11C C16C -66.5(3) . . . . ?
C16C C11C C12C C13C 2.6(4) . . . . ?
B1 C11C C12C C13C -175.7(2) . . . . ?
C11C C12C C13C C14C -0.1(4) . . . . ?
C12C C13C C14C C15C -1.7(4) . . . . ?
C13C C14C C15C C16C 1.0(4) . . . . ?
C14C C15C C16C C11C 1.6(4) . . . . ?
C12C C11C C16C C15C -3.3(4) . . . . ?
B1 C11C C16C C15C 175.0(2) . . . . ?
C41C B1 C21C C22C -96.1(3) . . . . ?
C11C B1 C21C C22C 24.2(3) . . . . ?
C31C B1 C21C C22C 146.2(2) . . . . ?
C41C B1 C21C C26C 81.6(3) . . . . ?
C11C B1 C21C C26C -158.1(2) . . . . ?
C31C B1 C21C C26C -36.1(3) . . . . ?
C26C C21C C22C C23C -0.3(4) . . . . ?
B1 C21C C22C C23C 177.6(2) . . . . ?
C21C C22C C23C C24C 0.3(4) . . . . ?
C22C C23C C24C C25C -0.1(4) . . . . ?
C23C C24C C25C C26C -0.3(4) . . . . ?
C24C C25C C26C C21C 0.3(4) . . . . ?
C22C C21C C26C C25C -0.1(4) . . . . ?
B1 C21C C26C C25C -177.9(2) . . . . ?
C41C B1 C31C C36C -40.0(3) . . . . ?
C11C B1 C31C C36C -159.3(2) . . . . ?
C21C B1 C31C C36C 79.0(3) . . . . ?
C41C B1 C31C C32C 141.7(2) . . . . ?
C11C B1 C31C C32C 22.4(3) . . . . ?
C21C B1 C31C C32C -99.4(3) . . . . ?
C36C C31C C32C C33C 1.1(4) . . . . ?
B1 C31C C32C C33C 179.5(2) . . . . ?
C31C C32C C33C C34C -1.2(4) . . . . ?
C32C C33C C34C C35C 0.1(5) . . . . ?
C33C C34C C35C C36C 0.9(5) . . . . ?
C34C C35C C36C C31C -0.9(5) . . . . ?
C32C C31C C36C C35C -0.1(4) . . . . ?
B1 C31C C36C C35C -178.6(3) . . . . ?
C11C B1 C41C C42C -113.7(3) . . . . ?
C21C B1 C41C C42C 7.4(3) . . . . ?
C31C B1 C41C C42C 125.8(2) . . . . ?
C11C B1 C41C C46C 63.7(3) . . . . ?
C21C B1 C41C C46C -175.2(2) . . . . ?
C31C B1 C41C C46C -56.8(3) . . . . ?
C46C C41C C42C C43C -1.9(4) . . . . ?
B1 C41C C42C C43C 175.6(2) . . . . ?
C41C C42C C43C C44C 0.6(4) . . . . ?
C42C C43C C44C C45C 0.8(4) . . . . ?
C43C C44C C45C C46C -0.6(4) . . . . ?
C44C C45C C46C C41C -0.9(4) . . . . ?
C42C C41C C46C C45C 2.1(4) . . . . ?
B1 C41C C46C C45C -175.6(2) . . . . ?
_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max 0.753
_refine_diff_density_min -0.802
_refine_diff_density_rms 0.064
_database_code_depnum_ccdc_archive 'CCDC 934043'
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_marina3_p1bar
#TrackingRef 'Marina3_Deposition_15Jun11.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C24 H30 Cl N5 Rh, C24 H20 B, C2 H2 Cl4'
_chemical_formula_sum 'C50 H52 B Cl5 N5 Rh'
_chemical_formula_weight 1013.94
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Triclinic
_symmetry_space_group_name_H-M P-1
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 11.3706(5)
_cell_length_b 12.6307(5)
_cell_length_c 17.3968(7)
_cell_angle_alpha 95.456(2)
_cell_angle_beta 101.823(2)
_cell_angle_gamma 104.458(2)
_cell_volume 2339.69(17)
_cell_formula_units_Z 2
_cell_measurement_temperature 156(2)
_cell_measurement_reflns_used 9964
_cell_measurement_theta_min 2.574
_cell_measurement_theta_max 30.439
_exptl_crystal_description Block
_exptl_crystal_colour 'Yellow orange'
_exptl_crystal_size_max 0.25
_exptl_crystal_size_mid 0.17
_exptl_crystal_size_min 0.08
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.439
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1044
_exptl_absorpt_coefficient_mu 0.692
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.8488
_exptl_absorpt_correction_T_max 0.9442
_exptl_absorpt_process_details 'SADABS (Bruker, 2001)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 156(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker kappa APEXII CCD Diffractometer'
_diffrn_measurement_method '\f scans, and \w scans with \k offsets'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 29804
_diffrn_reflns_av_R_equivalents 0.0297
_diffrn_reflns_av_sigmaI/netI 0.0246
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_theta_min 3.16
_diffrn_reflns_theta_max 25.00
_reflns_number_total 8053
_reflns_number_gt 7389
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2007)'
_computing_cell_refinement 'APEX2 (Bruker, 2007)'
_computing_data_reduction 'APEX2 (Bruker, 2007)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0213P)^2^+2.4051P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 8053
_refine_ls_number_parameters 565
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0282
_refine_ls_R_factor_gt 0.0247
_refine_ls_wR_factor_ref 0.0627
_refine_ls_wR_factor_gt 0.0603
_refine_ls_goodness_of_fit_ref 1.028
_refine_ls_restrained_S_all 1.028
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.714480(13) 0.727997(12) 0.732147(9) 0.01533(5) Uani 1 1 d . . .
Cl1 Cl 0.59514(4) 0.75520(4) 0.60791(3) 0.02096(11) Uani 1 1 d . . .
C1A C 0.87501(18) 0.71161(17) 0.81381(12) 0.0216(4) Uani 1 1 d . . .
C2A C 0.89201(18) 0.68184(17) 0.73486(13) 0.0227(4) Uani 1 1 d . . .
C3A C 0.89567(18) 0.77405(18) 0.69534(13) 0.0243(5) Uani 1 1 d . . .
C4A C 0.88085(18) 0.86296(17) 0.74840(12) 0.0222(4) Uani 1 1 d . . .
C5A C 0.87483(17) 0.82572(17) 0.82269(12) 0.0211(4) Uani 1 1 d . . .
C6A C 0.8775(2) 0.6398(2) 0.87754(14) 0.0338(5) Uani 1 1 d . . .
H6A1 H 0.9638 0.6392 0.8995 0.051 Uiso 1 1 calc R . .
H6A2 H 0.8265 0.5642 0.8549 0.051 Uiso 1 1 calc R . .
H6A3 H 0.8437 0.6689 0.9199 0.051 Uiso 1 1 calc R . .
C7A C 0.9087(2) 0.5734(2) 0.70376(16) 0.0363(6) Uani 1 1 d . . .
H7A1 H 0.8615 0.5503 0.6483 0.054 Uiso 1 1 calc R . .
H7A2 H 0.8780 0.5176 0.7357 0.054 Uiso 1 1 calc R . .
H7A3 H 0.9976 0.5814 0.7069 0.054 Uiso 1 1 calc R . .
C8A C 0.9116(2) 0.7815(2) 0.61277(14) 0.0383(6) Uani 1 1 d . . .
H8A1 H 0.9108 0.7088 0.5871 0.057 Uiso 1 1 calc R . .
H8A2 H 0.9914 0.8351 0.6146 0.057 Uiso 1 1 calc R . .
H8A3 H 0.8430 0.8056 0.5824 0.057 Uiso 1 1 calc R . .
C9A C 0.8909(2) 0.97664(19) 0.72870(16) 0.0351(6) Uani 1 1 d . . .
H9A1 H 0.8707 1.0214 0.7707 0.053 Uiso 1 1 calc R . .
H9A2 H 0.8323 0.9726 0.6779 0.053 Uiso 1 1 calc R . .
H9A3 H 0.9764 1.0107 0.7246 0.053 Uiso 1 1 calc R . .
C10A C 0.8727(2) 0.89303(19) 0.89767(13) 0.0325(5) Uani 1 1 d . . .
H10A H 0.9580 0.9218 0.9309 0.049 Uiso 1 1 calc R . .
H10C H 0.8201 0.8465 0.9266 0.049 Uiso 1 1 calc R . .
H10D H 0.8387 0.9549 0.8847 0.049 Uiso 1 1 calc R . .
N1B N 0.55031(15) 0.86264(14) 0.79275(10) 0.0219(4) Uani 1 1 d . . .
N2B N 0.52073(15) 0.70314(14) 0.82946(10) 0.0210(4) Uani 1 1 d . . .
N3B N 0.59909(14) 0.56743(13) 0.71633(9) 0.0173(3) Uani 1 1 d . . .
N4B N 0.58511(15) 0.49220(13) 0.65487(10) 0.0205(4) Uani 1 1 d . . .
N5B N 0.50637(15) 0.40090(13) 0.66702(10) 0.0216(4) Uani 1 1 d . . .
C1B C 0.58766(18) 0.76895(16) 0.78756(11) 0.0193(4) Uani 1 1 d . . .
C2B C 0.46227(19) 0.85505(18) 0.83810(13) 0.0259(5) Uani 1 1 d . . .
H2B H 0.4226 0.9102 0.8504 0.031 Uiso 1 1 calc R . .
C3B C 0.44374(19) 0.75542(18) 0.86121(12) 0.0255(5) Uani 1 1 d . . .
H3B H 0.3887 0.7262 0.8931 0.031 Uiso 1 1 calc R . .
C4B C 0.5324(2) 0.59278(17) 0.84237(12) 0.0241(4) Uani 1 1 d . . .
H4B1 H 0.4629 0.5547 0.8648 0.029 Uiso 1 1 calc R . .
H4B2 H 0.6119 0.6002 0.8814 0.029 Uiso 1 1 calc R . .
C5B C 0.53002(18) 0.52468(16) 0.76679(12) 0.0192(4) Uani 1 1 d . . .
C6B C 0.46973(19) 0.41704(17) 0.73477(12) 0.0223(4) Uani 1 1 d . . .
H6B H 0.4140 0.3649 0.7558 0.027 Uiso 1 1 calc R . .
C7B C 0.5916(2) 0.95801(18) 0.75399(15) 0.0320(5) Uani 1 1 d . . .
H7B1 H 0.6435 1.0209 0.7942 0.048 Uiso 1 1 calc R . .
H7B2 H 0.5186 0.9774 0.7247 0.048 Uiso 1 1 calc R . .
H7B3 H 0.6406 0.9398 0.7170 0.048 Uiso 1 1 calc R . .
C8B C 0.4766(2) 0.29803(17) 0.61134(14) 0.0292(5) Uani 1 1 d . . .
H8B1 H 0.4509 0.3130 0.5565 0.035 Uiso 1 1 calc R . .
H8B2 H 0.4052 0.2435 0.6223 0.035 Uiso 1 1 calc R . .
C9B C 0.5861(2) 0.24892(17) 0.61718(13) 0.0268(5) Uani 1 1 d . . .
C10B C 0.6947(2) 0.2879(2) 0.67622(15) 0.0351(5) Uani 1 1 d . . .
H10B H 0.7011 0.3458 0.7173 0.042 Uiso 1 1 calc R . .
C11B C 0.7949(3) 0.2435(2) 0.67628(18) 0.0464(7) Uani 1 1 d . . .
H11B H 0.8698 0.2721 0.7167 0.056 Uiso 1 1 calc R . .
C12B C 0.7861(3) 0.1588(2) 0.61848(19) 0.0508(8) Uani 1 1 d . . .
H12B H 0.8552 0.1295 0.6179 0.061 Uiso 1 1 calc R . .
C13B C 0.6763(3) 0.1161(2) 0.56111(18) 0.0521(8) Uani 1 1 d . . .
H13B H 0.6689 0.0554 0.5220 0.062 Uiso 1 1 calc R . .
C14B C 0.5763(3) 0.1610(2) 0.55989(15) 0.0400(6) Uani 1 1 d . . .
H14B H 0.5011 0.1315 0.5198 0.048 Uiso 1 1 calc R . .
B1 B 0.2797(2) 0.17325(19) 0.84007(14) 0.0198(5) Uani 1 1 d . . .
C11C C 0.18506(18) 0.24193(17) 0.86608(12) 0.0204(4) Uani 1 1 d . . .
C12C C 0.08306(19) 0.19389(18) 0.89651(12) 0.0245(4) Uani 1 1 d . . .
H12C H 0.0711 0.1197 0.9063 0.029 Uiso 1 1 calc R . .
C13C C -0.0015(2) 0.2504(2) 0.91300(14) 0.0339(5) Uani 1 1 d . . .
H13C H -0.0700 0.2141 0.9331 0.041 Uiso 1 1 calc R . .
C14C C 0.0133(2) 0.3587(2) 0.90041(14) 0.0357(6) Uani 1 1 d . . .
H14C H -0.0443 0.3974 0.9119 0.043 Uiso 1 1 calc R . .
C15C C 0.1131(2) 0.40990(19) 0.87090(14) 0.0329(5) Uani 1 1 d . . .
H15C H 0.1248 0.4844 0.8619 0.040 Uiso 1 1 calc R . .
C16C C 0.1965(2) 0.35203(18) 0.85439(14) 0.0278(5) Uani 1 1 d . . .
H16C H 0.2646 0.3889 0.8342 0.033 Uiso 1 1 calc R . .
C21C C 0.42710(18) 0.24810(16) 0.87384(11) 0.0183(4) Uani 1 1 d . . .
C22C C 0.46511(19) 0.33407(17) 0.93832(12) 0.0223(4) Uani 1 1 d . . .
H22C H 0.4033 0.3518 0.9625 0.027 Uiso 1 1 calc R . .
C23C C 0.5894(2) 0.39479(17) 0.96876(13) 0.0252(5) Uani 1 1 d . . .
H23C H 0.6102 0.4536 1.0118 0.030 Uiso 1 1 calc R . .
C24C C 0.68260(19) 0.36978(18) 0.93653(13) 0.0264(5) Uani 1 1 d . . .
H24C H 0.7676 0.4108 0.9571 0.032 Uiso 1 1 calc R . .
C25C C 0.6495(2) 0.28375(19) 0.87371(13) 0.0279(5) Uani 1 1 d . . .
H25C H 0.7123 0.2646 0.8514 0.033 Uiso 1 1 calc R . .
C26C C 0.52475(19) 0.22536(17) 0.84320(12) 0.0236(4) Uani 1 1 d . . .
H26C H 0.5046 0.1674 0.7996 0.028 Uiso 1 1 calc R . .
C31C C 0.26625(18) 0.05844(16) 0.88047(12) 0.0201(4) Uani 1 1 d . . .
C32C C 0.3310(2) 0.05956(18) 0.95824(13) 0.0291(5) Uani 1 1 d . . .
H32C H 0.3842 0.1279 0.9878 0.035 Uiso 1 1 calc R . .
C33C C 0.3211(2) -0.03472(19) 0.99423(13) 0.0328(5) Uani 1 1 d . . .
H33C H 0.3669 -0.0296 1.0473 0.039 Uiso 1 1 calc R . .
C34C C 0.2451(2) -0.13604(18) 0.95337(14) 0.0272(5) Uani 1 1 d . . .
H34C H 0.2379 -0.2008 0.9777 0.033 Uiso 1 1 calc R . .
C35C C 0.18015(19) -0.14069(18) 0.87648(14) 0.0281(5) Uani 1 1 d . . .
H35C H 0.1282 -0.2096 0.8471 0.034 Uiso 1 1 calc R . .
C36C C 0.18985(18) -0.04546(17) 0.84150(13) 0.0253(5) Uani 1 1 d . . .
H36C H 0.1425 -0.0511 0.7888 0.030 Uiso 1 1 calc R . .
C41C C 0.24340(18) 0.14215(16) 0.74187(12) 0.0198(4) Uani 1 1 d . . .
C42C C 0.2825(2) 0.05843(18) 0.70333(13) 0.0270(5) Uani 1 1 d . . .
H42C H 0.3342 0.0224 0.7349 0.032 Uiso 1 1 calc R . .
C43C C 0.2492(2) 0.02614(19) 0.62173(14) 0.0346(5) Uani 1 1 d . . .
H43C H 0.2775 -0.0313 0.5988 0.042 Uiso 1 1 calc R . .
C44C C 0.1753(2) 0.0767(2) 0.57357(14) 0.0362(6) Uani 1 1 d . . .
H44C H 0.1518 0.0543 0.5176 0.043 Uiso 1 1 calc R . .
C45C C 0.1360(2) 0.1605(2) 0.60815(14) 0.0327(5) Uani 1 1 d . . .
H45C H 0.0863 0.1972 0.5757 0.039 Uiso 1 1 calc R . .
C46C C 0.16899(19) 0.19135(17) 0.69041(13) 0.0247(5) Uani 1 1 d . . .
H46C H 0.1396 0.2485 0.7126 0.030 Uiso 1 1 calc R . .
C1D C 0.2563(2) 0.66733(19) 0.57415(14) 0.0306(5) Uani 1 1 d . . .
H1D H 0.3182 0.7137 0.5490 0.037 Uiso 1 1 calc R . .
C2D C 0.2996(2) 0.56744(19) 0.59379(13) 0.0291(5) Uani 1 1 d . . .
H2D H 0.3824 0.5941 0.6330 0.035 Uiso 1 1 calc R . .
Cl1D Cl 0.10825(5) 0.63271(5) 0.50750(4) 0.04016(15) Uani 1 1 d . . .
Cl2D Cl 0.25510(6) 0.74672(6) 0.66409(4) 0.04824(17) Uani 1 1 d . . .
Cl3D Cl 0.19557(6) 0.47738(6) 0.63758(5) 0.04964(18) Uani 1 1 d . . .
Cl4D Cl 0.32150(6) 0.49796(6) 0.50770(4) 0.05138(18) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Rh1 0.01445(8) 0.01482(8) 0.01685(8) 0.00216(6) 0.00365(6) 0.00443(6)
Cl1 0.0172(2) 0.0262(3) 0.0171(2) 0.00606(19) -0.00088(18) 0.00471(19)
C1A 0.0163(10) 0.0218(10) 0.0239(11) 0.0045(9) 0.0002(8) 0.0036(8)
C2A 0.0127(9) 0.0246(11) 0.0294(11) 0.0008(9) 0.0031(8) 0.0054(8)
C3A 0.0133(9) 0.0344(12) 0.0256(11) 0.0065(9) 0.0046(8) 0.0065(9)
C4A 0.0137(9) 0.0224(11) 0.0288(11) 0.0076(9) 0.0020(8) 0.0033(8)
C5A 0.0144(9) 0.0205(10) 0.0243(11) 0.0018(8) 0.0005(8) 0.0013(8)
C6A 0.0302(12) 0.0323(13) 0.0369(13) 0.0173(11) 0.0004(10) 0.0069(10)
C7A 0.0283(12) 0.0327(13) 0.0482(15) -0.0033(11) 0.0058(11) 0.0154(10)
C8A 0.0292(12) 0.0611(17) 0.0283(12) 0.0129(12) 0.0136(10) 0.0116(12)
C9A 0.0223(11) 0.0280(12) 0.0544(15) 0.0202(11) 0.0059(11) 0.0032(9)
C10A 0.0326(12) 0.0302(12) 0.0282(12) -0.0049(10) 0.0035(10) 0.0037(10)
N1B 0.0217(9) 0.0193(9) 0.0254(9) 0.0000(7) 0.0050(7) 0.0086(7)
N2B 0.0245(9) 0.0216(9) 0.0200(9) 0.0019(7) 0.0088(7) 0.0094(7)
N3B 0.0178(8) 0.0168(8) 0.0181(8) 0.0021(7) 0.0057(7) 0.0051(7)
N4B 0.0216(9) 0.0176(9) 0.0216(9) 0.0005(7) 0.0066(7) 0.0040(7)
N5B 0.0218(9) 0.0148(8) 0.0270(9) 0.0011(7) 0.0069(7) 0.0031(7)
C1B 0.0185(10) 0.0185(10) 0.0193(10) -0.0009(8) 0.0019(8) 0.0058(8)
C2B 0.0246(11) 0.0278(12) 0.0274(11) -0.0034(9) 0.0062(9) 0.0138(9)
C3B 0.0251(11) 0.0324(12) 0.0228(11) 0.0003(9) 0.0104(9) 0.0126(9)
C4B 0.0315(11) 0.0245(11) 0.0216(10) 0.0063(9) 0.0121(9) 0.0115(9)
C5B 0.0196(10) 0.0200(10) 0.0218(10) 0.0071(8) 0.0076(8) 0.0089(8)
C6B 0.0217(10) 0.0197(10) 0.0292(11) 0.0082(9) 0.0106(9) 0.0069(8)
C7B 0.0332(12) 0.0205(11) 0.0476(14) 0.0075(10) 0.0146(11) 0.0119(9)
C8B 0.0316(12) 0.0177(11) 0.0325(12) -0.0054(9) 0.0059(10) 0.0015(9)
C9B 0.0406(13) 0.0169(10) 0.0274(11) 0.0066(9) 0.0154(10) 0.0089(9)
C10B 0.0412(14) 0.0285(12) 0.0376(13) 0.0041(10) 0.0102(11) 0.0130(11)
C11B 0.0439(15) 0.0421(16) 0.0631(18) 0.0213(14) 0.0167(13) 0.0214(12)
C12B 0.068(2) 0.0476(17) 0.068(2) 0.0363(16) 0.0430(17) 0.0400(15)
C13B 0.101(3) 0.0350(15) 0.0478(17) 0.0159(13) 0.0440(18) 0.0425(16)
C14B 0.0683(18) 0.0267(13) 0.0300(13) 0.0045(10) 0.0152(12) 0.0192(12)
B1 0.0203(11) 0.0188(11) 0.0226(12) 0.0037(9) 0.0076(9) 0.0072(9)
C11C 0.0184(10) 0.0223(11) 0.0193(10) -0.0015(8) 0.0037(8) 0.0059(8)
C12C 0.0229(11) 0.0278(11) 0.0217(10) 0.0013(9) 0.0051(8) 0.0063(9)
C13C 0.0234(11) 0.0505(15) 0.0315(12) 0.0038(11) 0.0126(10) 0.0128(10)
C14C 0.0288(12) 0.0470(15) 0.0370(13) -0.0031(11) 0.0081(10) 0.0238(11)
C15C 0.0319(12) 0.0269(12) 0.0406(13) -0.0011(10) 0.0040(10) 0.0155(10)
C16C 0.0227(11) 0.0256(11) 0.0369(13) 0.0035(10) 0.0102(9) 0.0078(9)
C21C 0.0219(10) 0.0164(10) 0.0196(10) 0.0072(8) 0.0071(8) 0.0073(8)
C22C 0.0235(10) 0.0214(10) 0.0250(11) 0.0054(9) 0.0102(9) 0.0074(8)
C23C 0.0287(11) 0.0203(11) 0.0238(11) 0.0015(9) 0.0046(9) 0.0035(9)
C24C 0.0206(10) 0.0276(12) 0.0287(11) 0.0095(9) 0.0031(9) 0.0027(9)
C25C 0.0212(11) 0.0356(13) 0.0328(12) 0.0097(10) 0.0114(9) 0.0131(9)
C26C 0.0246(11) 0.0239(11) 0.0238(11) 0.0015(9) 0.0064(9) 0.0099(9)
C31C 0.0186(10) 0.0210(10) 0.0258(11) 0.0053(8) 0.0117(8) 0.0086(8)
C32C 0.0422(13) 0.0210(11) 0.0226(11) 0.0005(9) 0.0087(10) 0.0061(10)
C33C 0.0473(14) 0.0318(13) 0.0213(11) 0.0077(10) 0.0105(10) 0.0115(11)
C34C 0.0267(11) 0.0253(11) 0.0384(13) 0.0150(10) 0.0178(10) 0.0114(9)
C35C 0.0171(10) 0.0211(11) 0.0449(14) 0.0077(10) 0.0061(9) 0.0033(8)
C36C 0.0173(10) 0.0242(11) 0.0329(12) 0.0074(9) 0.0013(9) 0.0060(8)
C41C 0.0168(9) 0.0176(10) 0.0241(10) 0.0036(8) 0.0066(8) 0.0017(8)
C42C 0.0297(12) 0.0251(11) 0.0264(11) 0.0021(9) 0.0058(9) 0.0094(9)
C43C 0.0484(15) 0.0261(12) 0.0282(12) -0.0014(10) 0.0114(11) 0.0085(11)
C44C 0.0466(15) 0.0323(13) 0.0216(11) -0.0008(10) 0.0039(10) 0.0013(11)
C45C 0.0319(12) 0.0352(13) 0.0289(12) 0.0118(10) 0.0029(10) 0.0066(10)
C46C 0.0242(11) 0.0222(11) 0.0287(11) 0.0066(9) 0.0078(9) 0.0062(9)
C1D 0.0236(11) 0.0324(13) 0.0324(12) 0.0054(10) 0.0045(9) 0.0033(9)
C2D 0.0236(11) 0.0326(12) 0.0291(12) 0.0019(10) 0.0037(9) 0.0071(9)
Cl1D 0.0309(3) 0.0501(4) 0.0375(3) 0.0116(3) -0.0021(2) 0.0140(3)
Cl2D 0.0447(4) 0.0407(4) 0.0515(4) -0.0141(3) 0.0027(3) 0.0127(3)
Cl3D 0.0407(4) 0.0457(4) 0.0687(5) 0.0330(4) 0.0151(3) 0.0123(3)
Cl4D 0.0411(4) 0.0665(5) 0.0422(4) -0.0182(3) 0.0012(3) 0.0240(3)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 C1B 2.0306(19) . ?
Rh1 N3B 2.0802(16) . ?
Rh1 C1A 2.1389(19) . ?
Rh1 C4A 2.155(2) . ?
Rh1 C5A 2.158(2) . ?
Rh1 C2A 2.2295(19) . ?
Rh1 C3A 2.237(2) . ?
Rh1 Cl1 2.4089(5) . ?
C1A C5A 1.435(3) . ?
C1A C2A 1.453(3) . ?
C1A C6A 1.498(3) . ?
C2A C3A 1.404(3) . ?
C2A C7A 1.495(3) . ?
C3A C4A 1.450(3) . ?
C3A C8A 1.493(3) . ?
C4A C5A 1.425(3) . ?
C4A C9A 1.490(3) . ?
C5A C10A 1.496(3) . ?
C6A H6A1 0.9800 . ?
C6A H6A2 0.9800 . ?
C6A H6A3 0.9800 . ?
C7A H7A1 0.9800 . ?
C7A H7A2 0.9800 . ?
C7A H7A3 0.9800 . ?
C8A H8A1 0.9800 . ?
C8A H8A2 0.9800 . ?
C8A H8A3 0.9800 . ?
C9A H9A1 0.9800 . ?
C9A H9A2 0.9800 . ?
C9A H9A3 0.9800 . ?
C10A H10A 0.9800 . ?
C10A H10C 0.9800 . ?
C10A H10D 0.9800 . ?
N1B C1B 1.355(3) . ?
N1B C2B 1.387(3) . ?
N1B C7B 1.459(3) . ?
N2B C1B 1.352(3) . ?
N2B C3B 1.388(3) . ?
N2B C4B 1.467(3) . ?
N3B N4B 1.316(2) . ?
N3B C5B 1.356(2) . ?
N4B N5B 1.336(2) . ?
N5B C6B 1.343(3) . ?
N5B C8B 1.466(3) . ?
C2B C3B 1.337(3) . ?
C2B H2B 0.9500 . ?
C3B H3B 0.9500 . ?
C4B C5B 1.493(3) . ?
C4B H4B1 0.9900 . ?
C4B H4B2 0.9900 . ?
C5B C6B 1.365(3) . ?
C6B H6B 0.9500 . ?
C7B H7B1 0.9800 . ?
C7B H7B2 0.9800 . ?
C7B H7B3 0.9800 . ?
C8B C9B 1.513(3) . ?
C8B H8B1 0.9900 . ?
C8B H8B2 0.9900 . ?
C9B C10B 1.380(3) . ?
C9B C14B 1.386(3) . ?
C10B C11B 1.390(3) . ?
C10B H10B 0.9500 . ?
C11B C12B 1.366(4) . ?
C11B H11B 0.9500 . ?
C12B C13B 1.377(5) . ?
C12B H12B 0.9500 . ?
C13B C14B 1.390(4) . ?
C13B H13B 0.9500 . ?
C14B H14B 0.9500 . ?
B1 C11C 1.645(3) . ?
B1 C41C 1.657(3) . ?
B1 C21C 1.657(3) . ?
B1 C31C 1.658(3) . ?
C11C C12C 1.398(3) . ?
C11C C16C 1.402(3) . ?
C12C C13C 1.390(3) . ?
C12C H12C 0.9500 . ?
C13C C14C 1.381(4) . ?
C13C H13C 0.9500 . ?
C14C C15C 1.380(3) . ?
C14C H14C 0.9500 . ?
C15C C16C 1.391(3) . ?
C15C H15C 0.9500 . ?
C16C H16C 0.9500 . ?
C21C C22C 1.400(3) . ?
C21C C26C 1.404(3) . ?
C22C C23C 1.393(3) . ?
C22C H22C 0.9500 . ?
C23C C24C 1.384(3) . ?
C23C H23C 0.9500 . ?
C24C C25C 1.385(3) . ?
C24C H24C 0.9500 . ?
C25C C26C 1.390(3) . ?
C25C H25C 0.9500 . ?
C26C H26C 0.9500 . ?
C31C C32C 1.399(3) . ?
C31C C36C 1.399(3) . ?
C32C C33C 1.388(3) . ?
C32C H32C 0.9500 . ?
C33C C34C 1.383(3) . ?
C33C H33C 0.9500 . ?
C34C C35C 1.377(3) . ?
C34C H34C 0.9500 . ?
C35C C36C 1.389(3) . ?
C35C H35C 0.9500 . ?
C36C H36C 0.9500 . ?
C41C C46C 1.401(3) . ?
C41C C42C 1.410(3) . ?
C42C C43C 1.385(3) . ?
C42C H42C 0.9500 . ?
C43C C44C 1.377(3) . ?
C43C H43C 0.9500 . ?
C44C C45C 1.381(3) . ?
C44C H44C 0.9500 . ?
C45C C46C 1.393(3) . ?
C45C H45C 0.9500 . ?
C46C H46C 0.9500 . ?
C1D C2D 1.508(3) . ?
C1D Cl1D 1.762(2) . ?
C1D Cl2D 1.781(2) . ?
C1D H1D 1.0000 . ?
C2D Cl4D 1.757(2) . ?
C2D Cl3D 1.771(2) . ?
C2D H2D 1.0000 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1B Rh1 N3B 84.65(7) . . ?
C1B Rh1 C1A 112.63(8) . . ?
N3B Rh1 C1A 99.79(7) . . ?
C1B Rh1 C4A 112.36(8) . . ?
N3B Rh1 C4A 160.25(7) . . ?
C1A Rh1 C4A 65.09(8) . . ?
C1B Rh1 C5A 94.56(8) . . ?
N3B Rh1 C5A 134.36(7) . . ?
C1A Rh1 C5A 39.02(8) . . ?
C4A Rh1 C5A 38.60(8) . . ?
C1B Rh1 C2A 151.30(8) . . ?
N3B Rh1 C2A 96.53(7) . . ?
C1A Rh1 C2A 38.79(8) . . ?
C4A Rh1 C2A 63.72(8) . . ?
C5A Rh1 C2A 64.24(8) . . ?
C1B Rh1 C3A 150.69(8) . . ?
N3B Rh1 C3A 124.51(7) . . ?
C1A Rh1 C3A 63.70(8) . . ?
C4A Rh1 C3A 38.50(8) . . ?
C5A Rh1 C3A 63.85(8) . . ?
C2A Rh1 C3A 36.63(8) . . ?
C1B Rh1 Cl1 89.36(6) . . ?
N3B Rh1 Cl1 89.56(5) . . ?
C1A Rh1 Cl1 156.67(6) . . ?
C4A Rh1 Cl1 100.21(5) . . ?
C5A Rh1 Cl1 136.08(6) . . ?
C2A Rh1 Cl1 119.28(6) . . ?
C3A Rh1 Cl1 93.37(5) . . ?
C5A C1A C2A 107.78(18) . . ?
C5A C1A C6A 126.73(19) . . ?
C2A C1A C6A 124.87(19) . . ?
C5A C1A Rh1 71.22(11) . . ?
C2A C1A Rh1 73.97(11) . . ?
C6A C1A Rh1 127.49(14) . . ?
C3A C2A C1A 107.95(18) . . ?
C3A C2A C7A 126.7(2) . . ?
C1A C2A C7A 125.3(2) . . ?
C3A C2A Rh1 71.99(11) . . ?
C1A C2A Rh1 67.23(11) . . ?
C7A C2A Rh1 128.44(15) . . ?
C2A C3A C4A 108.42(18) . . ?
C2A C3A C8A 126.8(2) . . ?
C4A C3A C8A 124.8(2) . . ?
C2A C3A Rh1 71.38(11) . . ?
C4A C3A Rh1 67.67(11) . . ?
C8A C3A Rh1 126.53(15) . . ?
C5A C4A C3A 107.93(17) . . ?
C5A C4A C9A 128.3(2) . . ?
C3A C4A C9A 123.2(2) . . ?
C5A C4A Rh1 70.84(11) . . ?
C3A C4A Rh1 73.83(11) . . ?
C9A C4A Rh1 128.15(14) . . ?
C4A C5A C1A 107.68(18) . . ?
C4A C5A C10A 126.82(19) . . ?
C1A C5A C10A 125.47(19) . . ?
C4A C5A Rh1 70.57(11) . . ?
C1A C5A Rh1 69.75(11) . . ?
C10A C5A Rh1 126.51(14) . . ?
C1A C6A H6A1 109.5 . . ?
C1A C6A H6A2 109.5 . . ?
H6A1 C6A H6A2 109.5 . . ?
C1A C6A H6A3 109.5 . . ?
H6A1 C6A H6A3 109.5 . . ?
H6A2 C6A H6A3 109.5 . . ?
C2A C7A H7A1 109.5 . . ?
C2A C7A H7A2 109.5 . . ?
H7A1 C7A H7A2 109.5 . . ?
C2A C7A H7A3 109.5 . . ?
H7A1 C7A H7A3 109.5 . . ?
H7A2 C7A H7A3 109.5 . . ?
C3A C8A H8A1 109.5 . . ?
C3A C8A H8A2 109.5 . . ?
H8A1 C8A H8A2 109.5 . . ?
C3A C8A H8A3 109.5 . . ?
H8A1 C8A H8A3 109.5 . . ?
H8A2 C8A H8A3 109.5 . . ?
C4A C9A H9A1 109.5 . . ?
C4A C9A H9A2 109.5 . . ?
H9A1 C9A H9A2 109.5 . . ?
C4A C9A H9A3 109.5 . . ?
H9A1 C9A H9A3 109.5 . . ?
H9A2 C9A H9A3 109.5 . . ?
C5A C10A H10A 109.5 . . ?
C5A C10A H10C 109.5 . . ?
H10A C10A H10C 109.5 . . ?
C5A C10A H10D 109.5 . . ?
H10A C10A H10D 109.5 . . ?
H10C C10A H10D 109.5 . . ?
C1B N1B C2B 110.82(17) . . ?
C1B N1B C7B 125.66(17) . . ?
C2B N1B C7B 123.48(17) . . ?
C1B N2B C3B 111.20(17) . . ?
C1B N2B C4B 124.16(16) . . ?
C3B N2B C4B 124.58(17) . . ?
N4B N3B C5B 110.57(16) . . ?
N4B N3B Rh1 123.48(12) . . ?
C5B N3B Rh1 125.94(13) . . ?
N3B N4B N5B 105.39(15) . . ?
N4B N5B C6B 112.00(16) . . ?
N4B N5B C8B 119.55(17) . . ?
C6B N5B C8B 128.33(17) . . ?
N2B C1B N1B 104.40(16) . . ?
N2B C1B Rh1 125.01(14) . . ?
N1B C1B Rh1 130.60(15) . . ?
C3B C2B N1B 107.05(18) . . ?
C3B C2B H2B 126.5 . . ?
N1B C2B H2B 126.5 . . ?
C2B C3B N2B 106.53(18) . . ?
C2B C3B H3B 126.7 . . ?
N2B C3B H3B 126.7 . . ?
N2B C4B C5B 111.44(16) . . ?
N2B C4B H4B1 109.3 . . ?
C5B C4B H4B1 109.3 . . ?
N2B C4B H4B2 109.3 . . ?
C5B C4B H4B2 109.3 . . ?
H4B1 C4B H4B2 108.0 . . ?
N3B C5B C6B 107.06(17) . . ?
N3B C5B C4B 121.01(18) . . ?
C6B C5B C4B 131.90(18) . . ?
N5B C6B C5B 104.97(17) . . ?
N5B C6B H6B 127.5 . . ?
C5B C6B H6B 127.5 . . ?
N1B C7B H7B1 109.5 . . ?
N1B C7B H7B2 109.5 . . ?
H7B1 C7B H7B2 109.5 . . ?
N1B C7B H7B3 109.5 . . ?
H7B1 C7B H7B3 109.5 . . ?
H7B2 C7B H7B3 109.5 . . ?
N5B C8B C9B 112.45(18) . . ?
N5B C8B H8B1 109.1 . . ?
C9B C8B H8B1 109.1 . . ?
N5B C8B H8B2 109.1 . . ?
C9B C8B H8B2 109.1 . . ?
H8B1 C8B H8B2 107.8 . . ?
C10B C9B C14B 118.8(2) . . ?
C10B C9B C8B 123.2(2) . . ?
C14B C9B C8B 118.0(2) . . ?
C9B C10B C11B 120.7(2) . . ?
C9B C10B H10B 119.6 . . ?
C11B C10B H10B 119.6 . . ?
C12B C11B C10B 120.3(3) . . ?
C12B C11B H11B 119.9 . . ?
C10B C11B H11B 119.9 . . ?
C11B C12B C13B 119.5(2) . . ?
C11B C12B H12B 120.2 . . ?
C13B C12B H12B 120.2 . . ?
C12B C13B C14B 120.6(3) . . ?
C12B C13B H13B 119.7 . . ?
C14B C13B H13B 119.7 . . ?
C9B C14B C13B 120.0(3) . . ?
C9B C14B H14B 120.0 . . ?
C13B C14B H14B 120.0 . . ?
C11C B1 C41C 108.52(16) . . ?
C11C B1 C21C 110.20(16) . . ?
C41C B1 C21C 111.21(16) . . ?
C11C B1 C31C 110.57(16) . . ?
C41C B1 C31C 109.93(16) . . ?
C21C B1 C31C 106.43(16) . . ?
C12C C11C C16C 114.86(18) . . ?
C12C C11C B1 123.10(18) . . ?
C16C C11C B1 121.92(18) . . ?
C13C C12C C11C 122.6(2) . . ?
C13C C12C H12C 118.7 . . ?
C11C C12C H12C 118.7 . . ?
C14C C13C C12C 120.5(2) . . ?
C14C C13C H13C 119.7 . . ?
C12C C13C H13C 119.7 . . ?
C15C C14C C13C 119.0(2) . . ?
C15C C14C H14C 120.5 . . ?
C13C C14C H14C 120.5 . . ?
C14C C15C C16C 119.8(2) . . ?
C14C C15C H15C 120.1 . . ?
C16C C15C H15C 120.1 . . ?
C15C C16C C11C 123.2(2) . . ?
C15C C16C H16C 118.4 . . ?
C11C C16C H16C 118.4 . . ?
C22C C21C C26C 114.73(18) . . ?
C22C C21C B1 122.74(17) . . ?
C26C C21C B1 122.41(18) . . ?
C23C C22C C21C 123.05(19) . . ?
C23C C22C H22C 118.5 . . ?
C21C C22C H22C 118.5 . . ?
C24C C23C C22C 120.3(2) . . ?
C24C C23C H23C 119.9 . . ?
C22C C23C H23C 119.9 . . ?
C23C C24C C25C 118.64(19) . . ?
C23C C24C H24C 120.7 . . ?
C25C C24C H24C 120.7 . . ?
C24C C25C C26C 120.28(19) . . ?
C24C C25C H25C 119.9 . . ?
C26C C25C H25C 119.9 . . ?
C25C C26C C21C 123.0(2) . . ?
C25C C26C H26C 118.5 . . ?
C21C C26C H26C 118.5 . . ?
C32C C31C C36C 114.74(19) . . ?
C32C C31C B1 121.37(18) . . ?
C36C C31C B1 123.88(18) . . ?
C33C C32C C31C 122.9(2) . . ?
C33C C32C H32C 118.5 . . ?
C31C C32C H32C 118.5 . . ?
C34C C33C C32C 120.5(2) . . ?
C34C C33C H33C 119.8 . . ?
C32C C33C H33C 119.8 . . ?
C35C C34C C33C 118.4(2) . . ?
C35C C34C H34C 120.8 . . ?
C33C C34C H34C 120.8 . . ?
C34C C35C C36C 120.6(2) . . ?
C34C C35C H35C 119.7 . . ?
C36C C35C H35C 119.7 . . ?
C35C C36C C31C 122.9(2) . . ?
C35C C36C H36C 118.5 . . ?
C31C C36C H36C 118.5 . . ?
C46C C41C C42C 114.24(19) . . ?
C46C C41C B1 124.41(18) . . ?
C42C C41C B1 121.31(18) . . ?
C43C C42C C41C 123.2(2) . . ?
C43C C42C H42C 118.4 . . ?
C41C C42C H42C 118.4 . . ?
C44C C43C C42C 120.5(2) . . ?
C44C C43C H43C 119.8 . . ?
C42C C43C H43C 119.8 . . ?
C43C C44C C45C 118.7(2) . . ?
C43C C44C H44C 120.6 . . ?
C45C C44C H44C 120.6 . . ?
C44C C45C C46C 120.2(2) . . ?
C44C C45C H45C 119.9 . . ?
C46C C45C H45C 119.9 . . ?
C45C C46C C41C 123.1(2) . . ?
C45C C46C H46C 118.4 . . ?
C41C C46C H46C 118.4 . . ?
C2D C1D Cl1D 113.04(16) . . ?
C2D C1D Cl2D 108.82(16) . . ?
Cl1D C1D Cl2D 110.49(13) . . ?
C2D C1D H1D 108.1 . . ?
Cl1D C1D H1D 108.1 . . ?
Cl2D C1D H1D 108.1 . . ?
C1D C2D Cl4D 109.56(16) . . ?
C1D C2D Cl3D 112.32(16) . . ?
Cl4D C2D Cl3D 111.22(13) . . ?
C1D C2D H2D 107.9 . . ?
Cl4D C2D H2D 107.9 . . ?
Cl3D C2D H2D 107.9 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1B Rh1 C1A C5A -67.82(13) . . . . ?
N3B Rh1 C1A C5A -156.06(11) . . . . ?
C4A Rh1 C1A C5A 37.29(12) . . . . ?
C2A Rh1 C1A C5A 115.68(17) . . . . ?
C3A Rh1 C1A C5A 80.15(13) . . . . ?
Cl1 Rh1 C1A C5A 91.60(17) . . . . ?
C1B Rh1 C1A C2A 176.51(11) . . . . ?
N3B Rh1 C1A C2A 88.26(12) . . . . ?
C4A Rh1 C1A C2A -78.38(13) . . . . ?
C5A Rh1 C1A C2A -115.68(17) . . . . ?
C3A Rh1 C1A C2A -35.52(12) . . . . ?
Cl1 Rh1 C1A C2A -24.1(2) . . . . ?
C1B Rh1 C1A C6A 54.5(2) . . . . ?
N3B Rh1 C1A C6A -33.7(2) . . . . ?
C4A Rh1 C1A C6A 159.7(2) . . . . ?
C5A Rh1 C1A C6A 122.4(2) . . . . ?
C2A Rh1 C1A C6A -122.0(2) . . . . ?
C3A Rh1 C1A C6A -157.5(2) . . . . ?
Cl1 Rh1 C1A C6A -146.04(15) . . . . ?
C5A C1A C2A C3A -2.9(2) . . . . ?
C6A C1A C2A C3A -174.37(19) . . . . ?
Rh1 C1A C2A C3A 60.76(14) . . . . ?
C5A C1A C2A C7A 174.41(19) . . . . ?
C6A C1A C2A C7A 2.9(3) . . . . ?
Rh1 C1A C2A C7A -121.9(2) . . . . ?
C5A C1A C2A Rh1 -63.65(13) . . . . ?
C6A C1A C2A Rh1 124.9(2) . . . . ?
C1B Rh1 C2A C3A -125.93(17) . . . . ?
N3B Rh1 C2A C3A 143.30(12) . . . . ?
C1A Rh1 C2A C3A -119.20(17) . . . . ?
C4A Rh1 C2A C3A -36.99(12) . . . . ?
C5A Rh1 C2A C3A -80.14(13) . . . . ?
Cl1 Rh1 C2A C3A 50.12(13) . . . . ?
C1B Rh1 C2A C1A -6.7(2) . . . . ?
N3B Rh1 C2A C1A -97.51(12) . . . . ?
C4A Rh1 C2A C1A 82.21(13) . . . . ?
C5A Rh1 C2A C1A 39.06(12) . . . . ?
C3A Rh1 C2A C1A 119.20(17) . . . . ?
Cl1 Rh1 C2A C1A 169.32(10) . . . . ?
C1B Rh1 C2A C7A 111.1(2) . . . . ?
N3B Rh1 C2A C7A 20.3(2) . . . . ?
C1A Rh1 C2A C7A 117.8(2) . . . . ?
C4A Rh1 C2A C7A -159.9(2) . . . . ?
C5A Rh1 C2A C7A 156.9(2) . . . . ?
C3A Rh1 C2A C7A -123.0(3) . . . . ?
Cl1 Rh1 C2A C7A -72.8(2) . . . . ?
C1A C2A C3A C4A -0.1(2) . . . . ?
C7A C2A C3A C4A -177.37(19) . . . . ?
Rh1 C2A C3A C4A 57.67(13) . . . . ?
C1A C2A C3A C8A -179.9(2) . . . . ?
C7A C2A C3A C8A 2.8(3) . . . . ?
Rh1 C2A C3A C8A -122.2(2) . . . . ?
C1A C2A C3A Rh1 -57.79(13) . . . . ?
C7A C2A C3A Rh1 125.0(2) . . . . ?
C1B Rh1 C3A C2A 127.39(17) . . . . ?
N3B Rh1 C3A C2A -46.11(15) . . . . ?
C1A Rh1 C3A C2A 37.59(12) . . . . ?
C4A Rh1 C3A C2A 119.92(17) . . . . ?
C5A Rh1 C3A C2A 81.31(13) . . . . ?
Cl1 Rh1 C3A C2A -137.89(12) . . . . ?
C1B Rh1 C3A C4A 7.5(2) . . . . ?
N3B Rh1 C3A C4A -166.03(10) . . . . ?
C1A Rh1 C3A C4A -82.33(13) . . . . ?
C5A Rh1 C3A C4A -38.61(11) . . . . ?
C2A Rh1 C3A C4A -119.92(17) . . . . ?
Cl1 Rh1 C3A C4A 102.19(11) . . . . ?
C1B Rh1 C3A C8A -110.2(2) . . . . ?
N3B Rh1 C3A C8A 76.3(2) . . . . ?
C1A Rh1 C3A C8A 160.0(2) . . . . ?
C4A Rh1 C3A C8A -117.6(2) . . . . ?
C5A Rh1 C3A C8A -156.2(2) . . . . ?
C2A Rh1 C3A C8A 122.4(3) . . . . ?
Cl1 Rh1 C3A C8A -15.4(2) . . . . ?
C2A C3A C4A C5A 3.1(2) . . . . ?
C8A C3A C4A C5A -177.07(19) . . . . ?
Rh1 C3A C4A C5A 63.06(13) . . . . ?
C2A C3A C4A C9A 174.67(18) . . . . ?
C8A C3A C4A C9A -5.5(3) . . . . ?
Rh1 C3A C4A C9A -125.37(19) . . . . ?
C2A C3A C4A Rh1 -59.96(14) . . . . ?
C8A C3A C4A Rh1 119.9(2) . . . . ?
C1B Rh1 C4A C5A 67.83(13) . . . . ?
N3B Rh1 C4A C5A -80.0(2) . . . . ?
C1A Rh1 C4A C5A -37.70(12) . . . . ?
C2A Rh1 C4A C5A -80.89(13) . . . . ?
C3A Rh1 C4A C5A -116.11(16) . . . . ?
Cl1 Rh1 C4A C5A 161.38(11) . . . . ?
C1B Rh1 C4A C3A -176.05(11) . . . . ?
N3B Rh1 C4A C3A 36.1(3) . . . . ?
C1A Rh1 C4A C3A 78.41(12) . . . . ?
C5A Rh1 C4A C3A 116.11(16) . . . . ?
C2A Rh1 C4A C3A 35.22(11) . . . . ?
Cl1 Rh1 C4A C3A -82.51(11) . . . . ?
C1B Rh1 C4A C9A -56.3(2) . . . . ?
N3B Rh1 C4A C9A 155.9(2) . . . . ?
C1A Rh1 C4A C9A -161.8(2) . . . . ?
C5A Rh1 C4A C9A -124.1(3) . . . . ?
C2A Rh1 C4A C9A 155.0(2) . . . . ?
C3A Rh1 C4A C9A 119.8(3) . . . . ?
Cl1 Rh1 C4A C9A 37.3(2) . . . . ?
C3A C4A C5A C1A -4.9(2) . . . . ?
C9A C4A C5A C1A -175.87(19) . . . . ?
Rh1 C4A C5A C1A 60.16(13) . . . . ?
C3A C4A C5A C10A 173.38(19) . . . . ?
C9A C4A C5A C10A 2.4(3) . . . . ?
Rh1 C4A C5A C10A -121.6(2) . . . . ?
C3A C4A C5A Rh1 -65.02(13) . . . . ?
C9A C4A C5A Rh1 124.0(2) . . . . ?
C2A C1A C5A C4A 4.8(2) . . . . ?
C6A C1A C5A C4A 176.07(19) . . . . ?
Rh1 C1A C5A C4A -60.67(13) . . . . ?
C2A C1A C5A C10A -173.48(19) . . . . ?
C6A C1A C5A C10A -2.2(3) . . . . ?
Rh1 C1A C5A C10A 121.1(2) . . . . ?
C2A C1A C5A Rh1 65.46(13) . . . . ?
C6A C1A C5A Rh1 -123.3(2) . . . . ?
C1B Rh1 C5A C4A -120.77(12) . . . . ?
N3B Rh1 C5A C4A 152.26(11) . . . . ?
C1A Rh1 C5A C4A 118.25(17) . . . . ?
C2A Rh1 C5A C4A 79.43(13) . . . . ?
C3A Rh1 C5A C4A 38.51(12) . . . . ?
Cl1 Rh1 C5A C4A -26.94(15) . . . . ?
C1B Rh1 C5A C1A 120.97(12) . . . . ?
N3B Rh1 C5A C1A 34.00(16) . . . . ?
C4A Rh1 C5A C1A -118.25(17) . . . . ?
C2A Rh1 C5A C1A -38.83(12) . . . . ?
C3A Rh1 C5A C1A -79.74(13) . . . . ?
Cl1 Rh1 C5A C1A -145.19(10) . . . . ?
C1B Rh1 C5A C10A 1.20(19) . . . . ?
N3B Rh1 C5A C10A -85.8(2) . . . . ?
C1A Rh1 C5A C10A -119.8(2) . . . . ?
C4A Rh1 C5A C10A 122.0(2) . . . . ?
C2A Rh1 C5A C10A -158.6(2) . . . . ?
C3A Rh1 C5A C10A 160.5(2) . . . . ?
Cl1 Rh1 C5A C10A 95.04(19) . . . . ?
C1B Rh1 N3B N4B 148.71(15) . . . . ?
C1A Rh1 N3B N4B -99.20(15) . . . . ?
C4A Rh1 N3B N4B -60.9(3) . . . . ?
C5A Rh1 N3B N4B -120.13(15) . . . . ?
C2A Rh1 N3B N4B -60.13(15) . . . . ?
C3A Rh1 N3B N4B -34.48(17) . . . . ?
Cl1 Rh1 N3B N4B 59.31(14) . . . . ?
C1B Rh1 N3B C5B -32.32(16) . . . . ?
C1A Rh1 N3B C5B 79.77(16) . . . . ?
C4A Rh1 N3B C5B 118.1(2) . . . . ?
C5A Rh1 N3B C5B 58.84(19) . . . . ?
C2A Rh1 N3B C5B 118.84(16) . . . . ?
C3A Rh1 N3B C5B 144.49(15) . . . . ?
Cl1 Rh1 N3B C5B -121.72(15) . . . . ?
C5B N3B N4B N5B -0.1(2) . . . . ?
Rh1 N3B N4B N5B 178.99(12) . . . . ?
N3B N4B N5B C6B 0.3(2) . . . . ?
N3B N4B N5B C8B -176.14(17) . . . . ?
C3B N2B C1B N1B -0.7(2) . . . . ?
C4B N2B C1B N1B -178.24(18) . . . . ?
C3B N2B C1B Rh1 178.93(14) . . . . ?
C4B N2B C1B Rh1 1.4(3) . . . . ?
C2B N1B C1B N2B 0.6(2) . . . . ?
C7B N1B C1B N2B -177.07(19) . . . . ?
C2B N1B C1B Rh1 -178.99(15) . . . . ?
C7B N1B C1B Rh1 3.3(3) . . . . ?
N3B Rh1 C1B N2B 31.90(16) . . . . ?
C1A Rh1 C1B N2B -66.49(18) . . . . ?
C4A Rh1 C1B N2B -137.71(16) . . . . ?
C5A Rh1 C1B N2B -102.29(17) . . . . ?
C2A Rh1 C1B N2B -61.9(2) . . . . ?
C3A Rh1 C1B N2B -142.73(16) . . . . ?
Cl1 Rh1 C1B N2B 121.51(16) . . . . ?
N3B Rh1 C1B N1B -148.54(19) . . . . ?
C1A Rh1 C1B N1B 113.07(18) . . . . ?
C4A Rh1 C1B N1B 41.9(2) . . . . ?
C5A Rh1 C1B N1B 77.27(19) . . . . ?
C2A Rh1 C1B N1B 117.6(2) . . . . ?
C3A Rh1 C1B N1B 36.8(3) . . . . ?
Cl1 Rh1 C1B N1B -58.93(18) . . . . ?
C1B N1B C2B C3B -0.3(2) . . . . ?
C7B N1B C2B C3B 177.4(2) . . . . ?
N1B C2B C3B N2B -0.1(2) . . . . ?
C1B N2B C3B C2B 0.5(2) . . . . ?
C4B N2B C3B C2B 178.05(19) . . . . ?
C1B N2B C4B C5B -47.4(3) . . . . ?
C3B N2B C4B C5B 135.4(2) . . . . ?
N4B N3B C5B C6B -0.1(2) . . . . ?
Rh1 N3B C5B C6B -179.19(13) . . . . ?
N4B N3B C5B C4B 178.38(17) . . . . ?
Rh1 N3B C5B C4B -0.7(3) . . . . ?
N2B C4B C5B N3B 45.9(3) . . . . ?
N2B C4B C5B C6B -136.1(2) . . . . ?
N4B N5B C6B C5B -0.4(2) . . . . ?
C8B N5B C6B C5B 175.69(19) . . . . ?
N3B C5B C6B N5B 0.3(2) . . . . ?
C4B C5B C6B N5B -178.0(2) . . . . ?
N4B N5B C8B C9B 70.2(2) . . . . ?
C6B N5B C8B C9B -105.6(2) . . . . ?
N5B C8B C9B C10B 9.0(3) . . . . ?
N5B C8B C9B C14B -170.57(19) . . . . ?
C14B C9B C10B C11B 3.0(3) . . . . ?
C8B C9B C10B C11B -176.5(2) . . . . ?
C9B C10B C11B C12B -1.3(4) . . . . ?
C10B C11B C12B C13B -1.4(4) . . . . ?
C11B C12B C13B C14B 2.3(4) . . . . ?
C10B C9B C14B C13B -2.1(3) . . . . ?
C8B C9B C14B C13B 177.5(2) . . . . ?
C12B C13B C14B C9B -0.6(4) . . . . ?
C41C B1 C11C C12C 102.6(2) . . . . ?
C21C B1 C11C C12C -135.41(19) . . . . ?
C31C B1 C11C C12C -18.0(3) . . . . ?
C41C B1 C11C C16C -73.2(2) . . . . ?
C21C B1 C11C C16C 48.8(3) . . . . ?
C31C B1 C11C C16C 166.16(19) . . . . ?
C16C C11C C12C C13C 0.8(3) . . . . ?
B1 C11C C12C C13C -175.3(2) . . . . ?
C11C C12C C13C C14C -0.7(3) . . . . ?
C12C C13C C14C C15C 0.2(4) . . . . ?
C13C C14C C15C C16C 0.0(4) . . . . ?
C14C C15C C16C C11C 0.1(4) . . . . ?
C12C C11C C16C C15C -0.5(3) . . . . ?
B1 C11C C16C C15C 175.6(2) . . . . ?
C11C B1 C21C C22C 22.4(3) . . . . ?
C41C B1 C21C C22C 142.80(18) . . . . ?
C31C B1 C21C C22C -97.5(2) . . . . ?
C11C B1 C21C C26C -161.86(18) . . . . ?
C41C B1 C21C C26C -41.5(2) . . . . ?
C31C B1 C21C C26C 78.2(2) . . . . ?
C26C C21C C22C C23C 1.7(3) . . . . ?
B1 C21C C22C C23C 177.71(19) . . . . ?
C21C C22C C23C C24C -1.6(3) . . . . ?
C22C C23C C24C C25C 0.1(3) . . . . ?
C23C C24C C25C C26C 1.0(3) . . . . ?
C24C C25C C26C C21C -0.9(3) . . . . ?
C22C C21C C26C C25C -0.5(3) . . . . ?
B1 C21C C26C C25C -176.52(19) . . . . ?
C11C B1 C31C C32C -83.3(2) . . . . ?
C41C B1 C31C C32C 156.91(18) . . . . ?
C21C B1 C31C C32C 36.4(2) . . . . ?
C11C B1 C31C C36C 95.8(2) . . . . ?
C41C B1 C31C C36C -24.0(3) . . . . ?
C21C B1 C31C C36C -144.53(19) . . . . ?
C36C C31C C32C C33C 0.2(3) . . . . ?
B1 C31C C32C C33C 179.4(2) . . . . ?
C31C C32C C33C C34C 0.2(4) . . . . ?
C32C C33C C34C C35C 0.1(3) . . . . ?
C33C C34C C35C C36C -0.8(3) . . . . ?
C34C C35C C36C C31C 1.3(3) . . . . ?
C32C C31C C36C C35C -1.0(3) . . . . ?
B1 C31C C36C C35C 179.88(19) . . . . ?
C11C B1 C41C C46C 15.5(3) . . . . ?
C21C B1 C41C C46C -105.8(2) . . . . ?
C31C B1 C41C C46C 136.57(19) . . . . ?
C11C B1 C41C C42C -161.80(18) . . . . ?
C21C B1 C41C C42C 76.8(2) . . . . ?
C31C B1 C41C C42C -40.8(2) . . . . ?
C46C C41C C42C C43C -0.8(3) . . . . ?
B1 C41C C42C C43C 176.8(2) . . . . ?
C41C C42C C43C C44C 0.6(4) . . . . ?
C42C C43C C44C C45C 0.4(4) . . . . ?
C43C C44C C45C C46C -1.2(3) . . . . ?
C44C C45C C46C C41C 0.9(3) . . . . ?
C42C C41C C46C C45C 0.1(3) . . . . ?
B1 C41C C46C C45C -177.42(19) . . . . ?
Cl1D C1D C2D Cl4D 64.67(19) . . . . ?
Cl2D C1D C2D Cl4D -172.18(11) . . . . ?
Cl1D C1D C2D Cl3D -59.5(2) . . . . ?
Cl2D C1D C2D Cl3D 63.69(18) . . . . ?
_diffrn_measured_fraction_theta_max 0.976
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.976
_refine_diff_density_max 0.524
_refine_diff_density_min -0.561
_refine_diff_density_rms 0.052
_database_code_depnum_ccdc_archive 'CCDC 934044'
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_marina4
#TrackingRef 'Marina4_Deposition_04Jul12.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C23 H28 Cl N5 Rh, C24 H20 B'
_chemical_formula_sum 'C47 H48 B Cl N5 Rh'
_chemical_formula_weight 832.07
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M 'P 21/n'
_symmetry_space_group_name_Hall '-P 2yn '
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 12.3833(9)
_cell_length_b 24.7571(17)
_cell_length_c 13.1128(9)
_cell_angle_alpha 90.00
_cell_angle_beta 92.980(2)
_cell_angle_gamma 90.00
_cell_volume 4014.6(5)
_cell_formula_units_Z 4
_cell_measurement_temperature 160(2)
_cell_measurement_reflns_used 9102
_cell_measurement_theta_min 2.847
_cell_measurement_theta_max 30.008
_exptl_crystal_description 'Square plates'
_exptl_crystal_colour Yellow
_exptl_crystal_size_max 0.28
_exptl_crystal_size_mid 0.25
_exptl_crystal_size_min 0.09
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.377
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1728
_exptl_absorpt_coefficient_mu 0.532
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.8657
_exptl_absorpt_correction_T_max 0.9551
_exptl_absorpt_process_details 'SADABS (Bruker, 2001)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 160(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker kappa APEXII CCD Diffractometer'
_diffrn_measurement_method '\f scans, and \w scans with \k offsets'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 30243
_diffrn_reflns_av_R_equivalents 0.0436
_diffrn_reflns_av_sigmaI/netI 0.0331
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_k_max 29
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_theta_min 2.21
_diffrn_reflns_theta_max 25.00
_reflns_number_total 7047
_reflns_number_gt 5955
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2007)'
_computing_cell_refinement 'APEX2 (Bruker, 2007)'
_computing_data_reduction 'APEX2 (Bruker, 2007)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+0.7731P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 7047
_refine_ls_number_parameters 502
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0353
_refine_ls_R_factor_gt 0.0273
_refine_ls_wR_factor_ref 0.0716
_refine_ls_wR_factor_gt 0.0686
_refine_ls_goodness_of_fit_ref 1.039
_refine_ls_restrained_S_all 1.039
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.776096(11) 0.925938(6) 0.751331(12) 0.01915(7) Uani 1 1 d . . .
Cl2 Cl 0.80738(4) 1.01524(2) 0.81957(4) 0.02625(13) Uani 1 1 d . . .
N1 N 0.92979(12) 0.89481(7) 0.93287(14) 0.0252(4) Uani 1 1 d . . .
C2 C 0.83128(15) 0.89157(8) 0.88387(16) 0.0224(5) Uani 1 1 d . . .
N3 N 0.77519(13) 0.85702(7) 0.94137(13) 0.0243(4) Uani 1 1 d . . .
C4 C 0.83927(16) 0.83857(9) 1.02428(18) 0.0302(5) Uani 1 1 d . . .
H4 H 0.8186 0.8140 1.0753 0.036 Uiso 1 1 calc R . .
C5 C 0.93522(17) 0.86215(9) 1.01803(18) 0.0306(5) Uani 1 1 d . . .
H5 H 0.9964 0.8573 1.0639 0.037 Uiso 1 1 calc R . .
C6 C 1.01587(17) 0.93173(9) 0.90616(19) 0.0324(6) Uani 1 1 d . . .
H6A H 1.0701 0.9120 0.8691 0.049 Uiso 1 1 calc R . .
H6B H 1.0500 0.9473 0.9686 0.049 Uiso 1 1 calc R . .
H6C H 0.9853 0.9608 0.8628 0.049 Uiso 1 1 calc R . .
N1' N 0.62844(13) 0.92519(7) 0.81788(13) 0.0220(4) Uani 1 1 d . . .
N2' N 0.55395(12) 0.96211(7) 0.79606(13) 0.0241(4) Uani 1 1 d . . .
N3' N 0.47025(12) 0.94875(7) 0.85257(13) 0.0226(4) Uani 1 1 d . . .
C4' C 0.49197(15) 0.90461(9) 0.91017(17) 0.0240(5) Uani 1 1 d . . .
H4' H 0.4463 0.8878 0.9567 0.029 Uiso 1 1 calc R . .
C5' C 0.59413(15) 0.88924(8) 0.88713(16) 0.0219(5) Uani 1 1 d . . .
C6' C 0.37355(15) 0.98065(8) 0.84219(16) 0.0230(5) Uani 1 1 d . . .
C7' C 0.34153(16) 1.00069(9) 0.74726(18) 0.0290(5) Uani 1 1 d . . .
H7' H 0.3827 0.9935 0.6897 0.035 Uiso 1 1 calc R . .
C8' C 0.24848(18) 1.03150(10) 0.73729(18) 0.0325(5) Uani 1 1 d . . .
H8' H 0.2257 1.0459 0.6726 0.039 Uiso 1 1 calc R . .
C9' C 0.18858(17) 1.04135(9) 0.82121(19) 0.0328(5) Uani 1 1 d . . .
H9' H 0.1244 1.0623 0.8140 0.039 Uiso 1 1 calc R . .
C10' C 0.22161(17) 1.02095(9) 0.91515(19) 0.0314(5) Uani 1 1 d . . .
H10' H 0.1797 1.0278 0.9724 0.038 Uiso 1 1 calc R . .
C11' C 0.31519(16) 0.99050(9) 0.92734(17) 0.0272(5) Uani 1 1 d . . .
H11' H 0.3387 0.9768 0.9924 0.033 Uiso 1 1 calc R . .
C1A C 0.66129(15) 0.84193(9) 0.92077(18) 0.0276(5) Uani 1 1 d . . .
H1A1 H 0.6324 0.8265 0.9834 0.033 Uiso 1 1 calc R . .
H1A2 H 0.6565 0.8138 0.8670 0.033 Uiso 1 1 calc R . .
C1B C 0.89005(17) 0.92954(9) 0.63313(17) 0.0288(5) Uani 1 1 d . . .
C2B C 0.78932(18) 0.95293(10) 0.59187(16) 0.0305(5) Uani 1 1 d . . .
C3B C 0.70948(18) 0.91236(10) 0.59378(17) 0.0315(5) Uani 1 1 d . . .
C4B C 0.75785(17) 0.86423(9) 0.63677(17) 0.0300(5) Uani 1 1 d . . .
C5B C 0.87131(16) 0.87478(9) 0.65654(17) 0.0295(5) Uani 1 1 d . . .
C6B C 0.99695(18) 0.95822(11) 0.6369(2) 0.0432(7) Uani 1 1 d . . .
H6B1 H 1.0507 0.9366 0.6763 0.065 Uiso 1 1 calc R . .
H6B2 H 0.9895 0.9935 0.6695 0.065 Uiso 1 1 calc R . .
H6B3 H 1.0204 0.9632 0.5673 0.065 Uiso 1 1 calc R . .
C7B C 0.7739(2) 1.00976(10) 0.55604(19) 0.0440(6) Uani 1 1 d . . .
H7B1 H 0.7935 1.0126 0.4848 0.066 Uiso 1 1 calc R . .
H7B2 H 0.8200 1.0339 0.5986 0.066 Uiso 1 1 calc R . .
H7B3 H 0.6980 1.0201 0.5612 0.066 Uiso 1 1 calc R . .
C8B C 0.5933(2) 0.91843(12) 0.5580(2) 0.0463(7) Uani 1 1 d . . .
H8B1 H 0.5838 0.9063 0.4869 0.069 Uiso 1 1 calc R . .
H8B2 H 0.5720 0.9565 0.5626 0.069 Uiso 1 1 calc R . .
H8B3 H 0.5480 0.8965 0.6010 0.069 Uiso 1 1 calc R . .
C9B C 0.7033(2) 0.81040(10) 0.6451(2) 0.0427(6) Uani 1 1 d . . .
H9B1 H 0.6284 0.8157 0.6635 0.064 Uiso 1 1 calc R . .
H9B2 H 0.7419 0.7887 0.6978 0.064 Uiso 1 1 calc R . .
H9B3 H 0.7041 0.7916 0.5794 0.064 Uiso 1 1 calc R . .
C10B C 0.95381(18) 0.83412(10) 0.6927(2) 0.0435(7) Uani 1 1 d . . .
H10A H 0.9779 0.8135 0.6342 0.065 Uiso 1 1 calc R . .
H10B H 0.9219 0.8095 0.7412 0.065 Uiso 1 1 calc R . .
H10C H 1.0158 0.8527 0.7263 0.065 Uiso 1 1 calc R . .
B1C B 0.72676(17) 0.25153(10) 0.17797(19) 0.0217(5) Uani 1 1 d . . .
C11C C 0.70070(15) 0.21308(8) 0.07745(16) 0.0213(4) Uani 1 1 d . . .
C12C C 0.76325(15) 0.16727(9) 0.05923(17) 0.0270(5) Uani 1 1 d . . .
H12C H 0.8170 0.1568 0.1097 0.032 Uiso 1 1 calc R . .
C13C C 0.75066(16) 0.13638(9) -0.02898(17) 0.0276(5) Uani 1 1 d . . .
H13C H 0.7963 0.1061 -0.0383 0.033 Uiso 1 1 calc R . .
C14C C 0.67198(16) 0.14965(9) -0.10299(17) 0.0262(5) Uani 1 1 d . . .
H14C H 0.6633 0.1290 -0.1639 0.031 Uiso 1 1 calc R . .
C15C C 0.60580(16) 0.19361(9) -0.08693(17) 0.0262(5) Uani 1 1 d . . .
H15C H 0.5503 0.2029 -0.1365 0.031 Uiso 1 1 calc R . .
C16C C 0.62044(15) 0.22417(8) 0.00151(16) 0.0227(5) Uani 1 1 d . . .
H16C H 0.5737 0.2540 0.0108 0.027 Uiso 1 1 calc R . .
C21C C 0.62249(15) 0.29193(8) 0.19111(16) 0.0226(5) Uani 1 1 d . . .
C22C C 0.60946(16) 0.33972(9) 0.13530(17) 0.0276(5) Uani 1 1 d . . .
H22C H 0.6647 0.3502 0.0917 0.033 Uiso 1 1 calc R . .
C23C C 0.51876(18) 0.37263(9) 0.14101(19) 0.0344(6) Uani 1 1 d . . .
H23C H 0.5130 0.4048 0.1016 0.041 Uiso 1 1 calc R . .
C24C C 0.43697(17) 0.35846(10) 0.20412(19) 0.0368(6) Uani 1 1 d . . .
H24C H 0.3757 0.3812 0.2094 0.044 Uiso 1 1 calc R . .
C25C C 0.44557(17) 0.31123(10) 0.25890(19) 0.0343(6) Uani 1 1 d . . .
H25C H 0.3892 0.3007 0.3011 0.041 Uiso 1 1 calc R . .
C26C C 0.53686(16) 0.27872(9) 0.25263(17) 0.0290(5) Uani 1 1 d . . .
H26C H 0.5413 0.2463 0.2915 0.035 Uiso 1 1 calc R . .
C31C C 0.69227(17) 0.16531(9) 0.29503(18) 0.0334(5) Uani 1 1 d . . .
H31C H 0.6465 0.1520 0.2402 0.040 Uiso 1 1 calc R . .
C32C C 0.70287(18) 0.13502(10) 0.38369(19) 0.0370(6) Uani 1 1 d . . .
H32C H 0.6652 0.1017 0.3884 0.044 Uiso 1 1 calc R . .
C33C C 0.76806(16) 0.15304(9) 0.46547(18) 0.0300(5) Uani 1 1 d . . .
H33C H 0.7755 0.1326 0.5267 0.036 Uiso 1 1 calc R . .
C34C C 0.82188(16) 0.20117(9) 0.45644(17) 0.0278(5) Uani 1 1 d . . .
H34C H 0.8668 0.2143 0.5119 0.033 Uiso 1 1 calc R . .
C35C C 0.81091(15) 0.23080(8) 0.36620(16) 0.0225(5) Uani 1 1 d . . .
H35C H 0.8498 0.2637 0.3617 0.027 Uiso 1 1 calc R . .
C36C C 0.74540(14) 0.21441(8) 0.28201(16) 0.0217(5) Uani 1 1 d . . .
C41C C 0.83882(15) 0.28681(9) 0.16197(16) 0.0241(5) Uani 1 1 d . . .
C42C C 0.85841(16) 0.33566(9) 0.21313(17) 0.0267(5) Uani 1 1 d . . .
H42C H 0.8037 0.3499 0.2536 0.032 Uiso 1 1 calc R . .
C43C C 0.95493(17) 0.36448(10) 0.20726(18) 0.0326(5) Uani 1 1 d . . .
H43C H 0.9649 0.3976 0.2432 0.039 Uiso 1 1 calc R . .
C44C C 1.03584(17) 0.34465(10) 0.14890(18) 0.0366(6) Uani 1 1 d . . .
H44C H 1.1019 0.3638 0.1448 0.044 Uiso 1 1 calc R . .
C45C C 1.01965(17) 0.29706(10) 0.09705(19) 0.0367(6) Uani 1 1 d . . .
H45C H 1.0747 0.2832 0.0565 0.044 Uiso 1 1 calc R . .
C46C C 0.92307(16) 0.26887(10) 0.10333(18) 0.0314(5) Uani 1 1 d . . .
H46C H 0.9139 0.2361 0.0663 0.038 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Rh1 0.01992(9) 0.01999(10) 0.01782(10) -0.00062(7) 0.00373(6) 0.00028(6)
Cl2 0.0352(3) 0.0188(3) 0.0249(3) -0.0020(2) 0.0036(2) -0.0002(2)
N1 0.0222(8) 0.0253(10) 0.0279(11) 0.0018(9) 0.0006(7) 0.0043(7)
C2 0.0246(10) 0.0189(11) 0.0241(12) -0.0009(10) 0.0047(9) 0.0040(8)
N3 0.0243(8) 0.0221(10) 0.0266(11) 0.0062(8) 0.0007(7) 0.0024(7)
C4 0.0351(11) 0.0277(13) 0.0279(13) 0.0102(11) 0.0019(10) 0.0077(10)
C5 0.0286(11) 0.0317(13) 0.0310(14) 0.0059(11) -0.0037(9) 0.0093(10)
C6 0.0240(10) 0.0320(14) 0.0411(15) 0.0049(11) 0.0010(10) -0.0006(9)
N1' 0.0228(8) 0.0220(10) 0.0214(10) 0.0033(8) 0.0034(7) 0.0027(7)
N2' 0.0220(8) 0.0258(10) 0.0249(10) 0.0054(8) 0.0066(7) 0.0034(7)
N3' 0.0193(8) 0.0234(10) 0.0255(10) 0.0021(8) 0.0050(7) -0.0007(7)
C4' 0.0247(10) 0.0235(12) 0.0242(12) 0.0033(10) 0.0039(9) -0.0027(9)
C5' 0.0226(9) 0.0204(11) 0.0228(12) 0.0023(10) 0.0020(8) -0.0018(8)
C6' 0.0208(9) 0.0192(11) 0.0292(13) 0.0004(10) 0.0030(9) 0.0005(8)
C7' 0.0291(11) 0.0319(13) 0.0263(13) -0.0010(11) 0.0037(9) 0.0021(9)
C8' 0.0334(11) 0.0300(13) 0.0336(14) 0.0017(11) -0.0038(10) 0.0046(10)
C9' 0.0274(11) 0.0282(13) 0.0424(15) -0.0054(12) -0.0008(10) 0.0059(9)
C10' 0.0295(11) 0.0287(13) 0.0366(14) -0.0060(11) 0.0084(10) 0.0045(9)
C11' 0.0294(10) 0.0257(12) 0.0266(13) -0.0003(10) 0.0038(9) -0.0010(9)
C1A 0.0264(10) 0.0241(12) 0.0323(13) 0.0060(10) 0.0024(9) -0.0017(9)
C1B 0.0315(11) 0.0365(14) 0.0195(12) -0.0048(10) 0.0121(9) -0.0042(10)
C2B 0.0402(12) 0.0361(14) 0.0156(12) -0.0017(10) 0.0053(9) -0.0037(11)
C3B 0.0359(12) 0.0426(15) 0.0159(12) -0.0079(11) 0.0018(9) -0.0030(10)
C4B 0.0347(11) 0.0308(13) 0.0251(13) -0.0103(11) 0.0068(10) -0.0027(10)
C5B 0.0316(11) 0.0328(14) 0.0249(13) -0.0116(11) 0.0095(9) 0.0022(10)
C6B 0.0380(13) 0.0576(18) 0.0353(15) -0.0025(13) 0.0150(11) -0.0149(12)
C7B 0.0632(16) 0.0421(16) 0.0269(14) 0.0085(12) 0.0030(12) -0.0031(13)
C8B 0.0381(13) 0.067(2) 0.0328(15) -0.0110(14) -0.0099(11) -0.0010(12)
C9B 0.0481(14) 0.0361(15) 0.0446(17) -0.0141(13) 0.0074(12) -0.0105(12)
C10B 0.0389(12) 0.0402(15) 0.0517(18) -0.0153(14) 0.0050(12) 0.0123(11)
B1C 0.0241(11) 0.0184(13) 0.0221(13) -0.0003(11) -0.0028(10) 0.0022(9)
C11C 0.0218(9) 0.0215(11) 0.0206(11) 0.0000(9) 0.0014(8) -0.0011(8)
C12C 0.0227(10) 0.0282(13) 0.0296(13) -0.0013(10) -0.0051(9) 0.0043(9)
C13C 0.0240(10) 0.0247(12) 0.0344(14) -0.0063(11) 0.0046(9) 0.0021(9)
C14C 0.0307(11) 0.0285(13) 0.0197(12) -0.0039(10) 0.0045(9) -0.0048(9)
C15C 0.0275(10) 0.0279(12) 0.0227(12) 0.0023(10) -0.0047(9) -0.0002(9)
C16C 0.0243(10) 0.0206(11) 0.0230(12) 0.0015(10) -0.0002(8) 0.0025(8)
C21C 0.0252(10) 0.0231(12) 0.0186(11) -0.0073(9) -0.0062(8) 0.0011(9)
C22C 0.0301(10) 0.0248(12) 0.0271(13) -0.0030(10) -0.0048(9) 0.0024(9)
C23C 0.0404(12) 0.0243(13) 0.0366(15) -0.0044(11) -0.0153(11) 0.0080(10)
C24C 0.0307(11) 0.0389(15) 0.0395(15) -0.0175(13) -0.0095(10) 0.0146(10)
C25C 0.0281(11) 0.0408(15) 0.0340(14) -0.0126(12) 0.0007(10) 0.0046(10)
C26C 0.0299(11) 0.0296(13) 0.0273(13) -0.0045(11) -0.0018(9) 0.0034(9)
C31C 0.0393(12) 0.0306(13) 0.0288(14) 0.0023(11) -0.0121(10) -0.0067(10)
C32C 0.0442(13) 0.0268(13) 0.0393(15) 0.0065(12) -0.0044(11) -0.0096(11)
C33C 0.0328(11) 0.0313(13) 0.0258(13) 0.0084(11) 0.0010(10) 0.0054(10)
C34C 0.0249(10) 0.0356(14) 0.0226(12) -0.0020(11) -0.0022(9) 0.0036(9)
C35C 0.0218(9) 0.0222(12) 0.0235(12) -0.0016(10) 0.0020(8) 0.0015(8)
C36C 0.0184(9) 0.0236(12) 0.0231(11) -0.0021(10) 0.0005(8) 0.0045(8)
C41C 0.0248(10) 0.0268(12) 0.0201(12) 0.0062(10) -0.0060(8) 0.0034(9)
C42C 0.0264(10) 0.0269(12) 0.0263(13) 0.0042(10) -0.0036(9) 0.0013(9)
C43C 0.0365(12) 0.0282(13) 0.0317(14) 0.0070(11) -0.0111(10) -0.0035(10)
C44C 0.0274(11) 0.0470(16) 0.0346(14) 0.0162(13) -0.0060(10) -0.0086(10)
C45C 0.0294(11) 0.0469(16) 0.0338(14) 0.0051(13) 0.0031(10) 0.0010(11)
C46C 0.0305(11) 0.0346(14) 0.0289(13) 0.0010(11) -0.0002(9) 0.0016(10)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 C2 2.022(2) . ?
Rh1 N1' 2.0666(16) . ?
Rh1 C4B 2.146(2) . ?
Rh1 C1B 2.152(2) . ?
Rh1 C5B 2.166(2) . ?
Rh1 C2B 2.209(2) . ?
Rh1 C3B 2.210(2) . ?
Rh1 Cl2 2.4088(6) . ?
N1 C2 1.351(3) . ?
N1 C5 1.378(3) . ?
N1 C6 1.461(3) . ?
C2 N3 1.355(3) . ?
N3 C4 1.389(3) . ?
N3 C1A 1.471(2) . ?
C4 C5 1.330(3) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
N1' N2' 1.319(2) . ?
N1' C5' 1.355(3) . ?
N2' N3' 1.346(2) . ?
N3' C4' 1.347(3) . ?
N3' C6' 1.435(2) . ?
C4' C5' 1.370(3) . ?
C4' H4' 0.9500 . ?
C5' C1A 1.490(3) . ?
C6' C7' 1.379(3) . ?
C6' C11' 1.383(3) . ?
C7' C8' 1.382(3) . ?
C7' H7' 0.9500 . ?
C8' C9' 1.380(3) . ?
C8' H8' 0.9500 . ?
C9' C10' 1.374(3) . ?
C9' H9' 0.9500 . ?
C10' C11' 1.385(3) . ?
C10' H10' 0.9500 . ?
C11' H11' 0.9500 . ?
C1A H1A1 0.9900 . ?
C1A H1A2 0.9900 . ?
C1B C5B 1.412(3) . ?
C1B C2B 1.454(3) . ?
C1B C6B 1.501(3) . ?
C2B C3B 1.410(3) . ?
C2B C7B 1.492(3) . ?
C3B C4B 1.436(3) . ?
C3B C8B 1.498(3) . ?
C4B C5B 1.439(3) . ?
C4B C9B 1.500(3) . ?
C5B C10B 1.494(3) . ?
C6B H6B1 0.9800 . ?
C6B H6B2 0.9800 . ?
C6B H6B3 0.9800 . ?
C7B H7B1 0.9800 . ?
C7B H7B2 0.9800 . ?
C7B H7B3 0.9800 . ?
C8B H8B1 0.9800 . ?
C8B H8B2 0.9800 . ?
C8B H8B3 0.9800 . ?
C9B H9B1 0.9800 . ?
C9B H9B2 0.9800 . ?
C9B H9B3 0.9800 . ?
C10B H10A 0.9800 . ?
C10B H10B 0.9800 . ?
C10B H10C 0.9800 . ?
B1C C11C 1.644(3) . ?
B1C C21C 1.649(3) . ?
B1C C36C 1.651(3) . ?
B1C C41C 1.662(3) . ?
C11C C16C 1.397(3) . ?
C11C C12C 1.401(3) . ?
C12C C13C 1.389(3) . ?
C12C H12C 0.9500 . ?
C13C C14C 1.379(3) . ?
C13C H13C 0.9500 . ?
C14C C15C 1.385(3) . ?
C14C H14C 0.9500 . ?
C15C C16C 1.389(3) . ?
C15C H15C 0.9500 . ?
C16C H16C 0.9500 . ?
C21C C22C 1.396(3) . ?
C21C C26C 1.404(3) . ?
C22C C23C 1.393(3) . ?
C22C H22C 0.9500 . ?
C23C C24C 1.386(3) . ?
C23C H23C 0.9500 . ?
C24C C25C 1.374(3) . ?
C24C H24C 0.9500 . ?
C25C C26C 1.394(3) . ?
C25C H25C 0.9500 . ?
C26C H26C 0.9500 . ?
C31C C32C 1.384(3) . ?
C31C C36C 1.397(3) . ?
C31C H31C 0.9500 . ?
C32C C33C 1.382(3) . ?
C32C H32C 0.9500 . ?
C33C C34C 1.373(3) . ?
C33C H33C 0.9500 . ?
C34C C35C 1.393(3) . ?
C34C H34C 0.9500 . ?
C35C C36C 1.396(3) . ?
C35C H35C 0.9500 . ?
C41C C42C 1.398(3) . ?
C41C C46C 1.400(3) . ?
C42C C43C 1.397(3) . ?
C42C H42C 0.9500 . ?
C43C C44C 1.382(3) . ?
C43C H43C 0.9500 . ?
C44C C45C 1.370(3) . ?
C44C H44C 0.9500 . ?
C45C C46C 1.391(3) . ?
C45C H45C 0.9500 . ?
C46C H46C 0.9500 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Rh1 N1' 84.27(7) . . ?
C2 Rh1 C4B 108.70(9) . . ?
N1' Rh1 C4B 103.06(7) . . ?
C2 Rh1 C1B 115.57(8) . . ?
N1' Rh1 C1B 158.81(8) . . ?
C4B Rh1 C1B 64.81(8) . . ?
C2 Rh1 C5B 94.44(8) . . ?
N1' Rh1 C5B 139.20(7) . . ?
C4B Rh1 C5B 38.99(8) . . ?
C1B Rh1 C5B 38.17(8) . . ?
C2 Rh1 C2B 154.48(8) . . ?
N1' Rh1 C2B 120.87(8) . . ?
C4B Rh1 C2B 64.10(9) . . ?
C1B Rh1 C2B 38.92(9) . . ?
C5B Rh1 C2B 64.18(9) . . ?
C2 Rh1 C3B 146.36(9) . . ?
N1' Rh1 C3B 95.62(8) . . ?
C4B Rh1 C3B 38.45(9) . . ?
C1B Rh1 C3B 63.88(8) . . ?
C5B Rh1 C3B 64.06(9) . . ?
C2B Rh1 C3B 37.22(8) . . ?
C2 Rh1 Cl2 91.51(6) . . ?
N1' Rh1 Cl2 88.86(5) . . ?
C4B Rh1 Cl2 157.27(6) . . ?
C1B Rh1 Cl2 97.51(6) . . ?
C5B Rh1 Cl2 131.91(6) . . ?
C2B Rh1 Cl2 93.18(6) . . ?
C3B Rh1 Cl2 122.13(7) . . ?
C2 N1 C5 110.82(17) . . ?
C2 N1 C6 125.11(18) . . ?
C5 N1 C6 123.80(18) . . ?
N1 C2 N3 104.42(18) . . ?
N1 C2 Rh1 129.80(15) . . ?
N3 C2 Rh1 125.72(15) . . ?
C2 N3 C4 110.76(17) . . ?
C2 N3 C1A 124.92(17) . . ?
C4 N3 C1A 124.30(17) . . ?
C5 C4 N3 106.45(19) . . ?
C5 C4 H4 126.8 . . ?
N3 C4 H4 126.8 . . ?
C4 C5 N1 107.54(19) . . ?
C4 C5 H5 126.2 . . ?
N1 C5 H5 126.2 . . ?
N1 C6 H6A 109.5 . . ?
N1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2' N1' C5' 111.11(16) . . ?
N2' N1' Rh1 121.74(13) . . ?
C5' N1' Rh1 127.15(13) . . ?
N1' N2' N3' 105.07(15) . . ?
N2' N3' C4' 111.76(15) . . ?
N2' N3' C6' 118.36(17) . . ?
C4' N3' C6' 129.85(16) . . ?
N3' C4' C5' 105.15(17) . . ?
N3' C4' H4' 127.4 . . ?
C5' C4' H4' 127.4 . . ?
N1' C5' C4' 106.90(18) . . ?
N1' C5' C1A 121.66(17) . . ?
C4' C5' C1A 131.36(19) . . ?
C7' C6' C11' 121.84(19) . . ?
C7' C6' N3' 118.88(18) . . ?
C11' C6' N3' 119.28(19) . . ?
C6' C7' C8' 118.9(2) . . ?
C6' C7' H7' 120.6 . . ?
C8' C7' H7' 120.6 . . ?
C9' C8' C7' 120.1(2) . . ?
C9' C8' H8' 119.9 . . ?
C7' C8' H8' 119.9 . . ?
C10' C9' C8' 120.2(2) . . ?
C10' C9' H9' 119.9 . . ?
C8' C9' H9' 119.9 . . ?
C9' C10' C11' 120.8(2) . . ?
C9' C10' H10' 119.6 . . ?
C11' C10' H10' 119.6 . . ?
C6' C11' C10' 118.2(2) . . ?
C6' C11' H11' 120.9 . . ?
C10' C11' H11' 120.9 . . ?
N3 C1A C5' 111.72(17) . . ?
N3 C1A H1A1 109.3 . . ?
C5' C1A H1A1 109.3 . . ?
N3 C1A H1A2 109.3 . . ?
C5' C1A H1A2 109.3 . . ?
H1A1 C1A H1A2 107.9 . . ?
C5B C1B C2B 108.40(19) . . ?
C5B C1B C6B 127.0(2) . . ?
C2B C1B C6B 124.2(2) . . ?
C5B C1B Rh1 71.46(12) . . ?
C2B C1B Rh1 72.69(12) . . ?
C6B C1B Rh1 127.35(16) . . ?
C3B C2B C1B 107.4(2) . . ?
C3B C2B C7B 126.8(2) . . ?
C1B C2B C7B 125.9(2) . . ?
C3B C2B Rh1 71.42(13) . . ?
C1B C2B Rh1 68.39(12) . . ?
C7B C2B Rh1 124.65(16) . . ?
C2B C3B C4B 108.6(2) . . ?
C2B C3B C8B 125.9(2) . . ?
C4B C3B C8B 125.5(2) . . ?
C2B C3B Rh1 71.36(13) . . ?
C4B C3B Rh1 68.37(13) . . ?
C8B C3B Rh1 125.70(16) . . ?
C3B C4B C5B 107.7(2) . . ?
C3B C4B C9B 125.8(2) . . ?
C5B C4B C9B 125.9(2) . . ?
C3B C4B Rh1 73.18(13) . . ?
C5B C4B Rh1 71.24(12) . . ?
C9B C4B Rh1 127.79(16) . . ?
C1B C5B C4B 107.8(2) . . ?
C1B C5B C10B 126.8(2) . . ?
C4B C5B C10B 125.4(2) . . ?
C1B C5B Rh1 70.36(12) . . ?
C4B C5B Rh1 69.77(11) . . ?
C10B C5B Rh1 126.57(17) . . ?
C1B C6B H6B1 109.5 . . ?
C1B C6B H6B2 109.5 . . ?
H6B1 C6B H6B2 109.5 . . ?
C1B C6B H6B3 109.5 . . ?
H6B1 C6B H6B3 109.5 . . ?
H6B2 C6B H6B3 109.5 . . ?
C2B C7B H7B1 109.5 . . ?
C2B C7B H7B2 109.5 . . ?
H7B1 C7B H7B2 109.5 . . ?
C2B C7B H7B3 109.5 . . ?
H7B1 C7B H7B3 109.5 . . ?
H7B2 C7B H7B3 109.5 . . ?
C3B C8B H8B1 109.5 . . ?
C3B C8B H8B2 109.5 . . ?
H8B1 C8B H8B2 109.5 . . ?
C3B C8B H8B3 109.5 . . ?
H8B1 C8B H8B3 109.5 . . ?
H8B2 C8B H8B3 109.5 . . ?
C4B C9B H9B1 109.5 . . ?
C4B C9B H9B2 109.5 . . ?
H9B1 C9B H9B2 109.5 . . ?
C4B C9B H9B3 109.5 . . ?
H9B1 C9B H9B3 109.5 . . ?
H9B2 C9B H9B3 109.5 . . ?
C5B C10B H10A 109.5 . . ?
C5B C10B H10B 109.5 . . ?
H10A C10B H10B 109.5 . . ?
C5B C10B H10C 109.5 . . ?
H10A C10B H10C 109.5 . . ?
H10B C10B H10C 109.5 . . ?
C11C B1C C21C 108.22(16) . . ?
C11C B1C C36C 110.69(17) . . ?
C21C B1C C36C 109.13(16) . . ?
C11C B1C C41C 109.47(16) . . ?
C21C B1C C41C 110.97(17) . . ?
C36C B1C C41C 108.36(16) . . ?
C16C C11C C12C 114.62(19) . . ?
C16C C11C B1C 124.09(18) . . ?
C12C C11C B1C 121.21(17) . . ?
C13C C12C C11C 123.28(19) . . ?
C13C C12C H12C 118.4 . . ?
C11C C12C H12C 118.4 . . ?
C14C C13C C12C 119.99(19) . . ?
C14C C13C H13C 120.0 . . ?
C12C C13C H13C 120.0 . . ?
C13C C14C C15C 118.8(2) . . ?
C13C C14C H14C 120.6 . . ?
C15C C14C H14C 120.6 . . ?
C14C C15C C16C 120.17(19) . . ?
C14C C15C H15C 119.9 . . ?
C16C C15C H15C 119.9 . . ?
C15C C16C C11C 123.05(19) . . ?
C15C C16C H16C 118.5 . . ?
C11C C16C H16C 118.5 . . ?
C22C C21C C26C 115.37(18) . . ?
C22C C21C B1C 121.93(18) . . ?
C26C C21C B1C 122.52(19) . . ?
C23C C22C C21C 122.6(2) . . ?
C23C C22C H22C 118.7 . . ?
C21C C22C H22C 118.7 . . ?
C24C C23C C22C 120.0(2) . . ?
C24C C23C H23C 120.0 . . ?
C22C C23C H23C 120.0 . . ?
C25C C24C C23C 119.2(2) . . ?
C25C C24C H24C 120.4 . . ?
C23C C24C H24C 120.4 . . ?
C24C C25C C26C 120.1(2) . . ?
C24C C25C H25C 119.9 . . ?
C26C C25C H25C 119.9 . . ?
C25C C26C C21C 122.6(2) . . ?
C25C C26C H26C 118.7 . . ?
C21C C26C H26C 118.7 . . ?
C32C C31C C36C 123.3(2) . . ?
C32C C31C H31C 118.3 . . ?
C36C C31C H31C 118.3 . . ?
C33C C32C C31C 120.2(2) . . ?
C33C C32C H32C 119.9 . . ?
C31C C32C H32C 119.9 . . ?
C34C C33C C32C 118.7(2) . . ?
C34C C33C H33C 120.7 . . ?
C32C C33C H33C 120.7 . . ?
C33C C34C C35C 120.3(2) . . ?
C33C C34C H34C 119.9 . . ?
C35C C34C H34C 119.9 . . ?
C34C C35C C36C 123.1(2) . . ?
C34C C35C H35C 118.5 . . ?
C36C C35C H35C 118.5 . . ?
C35C C36C C31C 114.48(19) . . ?
C35C C36C B1C 122.83(18) . . ?
C31C C36C B1C 122.61(18) . . ?
C42C C41C C46C 114.97(19) . . ?
C42C C41C B1C 121.28(18) . . ?
C46C C41C B1C 123.6(2) . . ?
C41C C42C C43C 122.9(2) . . ?
C41C C42C H42C 118.6 . . ?
C43C C42C H42C 118.6 . . ?
C44C C43C C42C 119.7(2) . . ?
C44C C43C H43C 120.1 . . ?
C42C C43C H43C 120.1 . . ?
C45C C44C C43C 119.3(2) . . ?
C45C C44C H44C 120.4 . . ?
C43C C44C H44C 120.4 . . ?
C44C C45C C46C 120.4(2) . . ?
C44C C45C H45C 119.8 . . ?
C46C C45C H45C 119.8 . . ?
C45C C46C C41C 122.7(2) . . ?
C45C C46C H46C 118.6 . . ?
C41C C46C H46C 118.6 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 C2 N3 1.1(2) . . . . ?
C6 N1 C2 N3 -173.17(19) . . . . ?
C5 N1 C2 Rh1 -176.08(15) . . . . ?
C6 N1 C2 Rh1 9.7(3) . . . . ?
N1' Rh1 C2 N1 -149.8(2) . . . . ?
C4B Rh1 C2 N1 108.38(19) . . . . ?
C1B Rh1 C2 N1 38.0(2) . . . . ?
C5B Rh1 C2 N1 71.2(2) . . . . ?
C2B Rh1 C2 N1 39.6(3) . . . . ?
C3B Rh1 C2 N1 118.7(2) . . . . ?
Cl2 Rh1 C2 N1 -61.05(19) . . . . ?
N1' Rh1 C2 N3 33.65(17) . . . . ?
C4B Rh1 C2 N3 -68.22(18) . . . . ?
C1B Rh1 C2 N3 -138.58(16) . . . . ?
C5B Rh1 C2 N3 -105.40(18) . . . . ?
C2B Rh1 C2 N3 -137.03(19) . . . . ?
C3B Rh1 C2 N3 -57.9(2) . . . . ?
Cl2 Rh1 C2 N3 122.36(17) . . . . ?
N1 C2 N3 C4 -0.8(2) . . . . ?
Rh1 C2 N3 C4 176.45(15) . . . . ?
N1 C2 N3 C1A 177.76(18) . . . . ?
Rh1 C2 N3 C1A -4.9(3) . . . . ?
C2 N3 C4 C5 0.3(2) . . . . ?
C1A N3 C4 C5 -178.3(2) . . . . ?
N3 C4 C5 N1 0.3(2) . . . . ?
C2 N1 C5 C4 -0.9(3) . . . . ?
C6 N1 C5 C4 173.4(2) . . . . ?
C2 Rh1 N1' N2' 149.85(17) . . . . ?
C4B Rh1 N1' N2' -102.24(16) . . . . ?
C1B Rh1 N1' N2' -49.9(3) . . . . ?
C5B Rh1 N1' N2' -119.98(17) . . . . ?
C2B Rh1 N1' N2' -34.81(18) . . . . ?
C3B Rh1 N1' N2' -63.95(17) . . . . ?
Cl2 Rh1 N1' N2' 58.22(15) . . . . ?
C2 Rh1 N1' C5' -29.81(18) . . . . ?
C4B Rh1 N1' C5' 78.10(19) . . . . ?
C1B Rh1 N1' C5' 130.5(2) . . . . ?
C5B Rh1 N1' C5' 60.4(2) . . . . ?
C2B Rh1 N1' C5' 145.53(17) . . . . ?
C3B Rh1 N1' C5' 116.39(18) . . . . ?
Cl2 Rh1 N1' C5' -121.44(17) . . . . ?
C5' N1' N2' N3' -0.5(2) . . . . ?
Rh1 N1' N2' N3' 179.82(12) . . . . ?
N1' N2' N3' C4' 0.9(2) . . . . ?
N1' N2' N3' C6' -177.51(17) . . . . ?
N2' N3' C4' C5' -0.9(2) . . . . ?
C6' N3' C4' C5' 177.2(2) . . . . ?
N2' N1' C5' C4' -0.1(2) . . . . ?
Rh1 N1' C5' C4' 179.63(14) . . . . ?
N2' N1' C5' C1A 176.99(19) . . . . ?
Rh1 N1' C5' C1A -3.3(3) . . . . ?
N3' C4' C5' N1' 0.6(2) . . . . ?
N3' C4' C5' C1A -176.1(2) . . . . ?
N2' N3' C6' C7' 36.3(3) . . . . ?
C4' N3' C6' C7' -141.7(2) . . . . ?
N2' N3' C6' C11' -143.67(19) . . . . ?
C4' N3' C6' C11' 38.3(3) . . . . ?
C11' C6' C7' C8' 0.0(3) . . . . ?
N3' C6' C7' C8' -179.9(2) . . . . ?
C6' C7' C8' C9' -0.7(3) . . . . ?
C7' C8' C9' C10' 0.5(4) . . . . ?
C8' C9' C10' C11' 0.2(4) . . . . ?
C7' C6' C11' C10' 0.7(3) . . . . ?
N3' C6' C11' C10' -179.37(19) . . . . ?
C9' C10' C11' C6' -0.8(3) . . . . ?
C2 N3 C1A C5' -40.6(3) . . . . ?
C4 N3 C1A C5' 137.8(2) . . . . ?
N1' C5' C1A N3 44.0(3) . . . . ?
C4' C5' C1A N3 -139.8(2) . . . . ?
C2 Rh1 C1B C5B 61.98(15) . . . . ?
N1' Rh1 C1B C5B -96.2(2) . . . . ?
C4B Rh1 C1B C5B -37.67(13) . . . . ?
C2B Rh1 C1B C5B -116.96(19) . . . . ?
C3B Rh1 C1B C5B -80.52(15) . . . . ?
Cl2 Rh1 C1B C5B 157.29(12) . . . . ?
C2 Rh1 C1B C2B 178.94(13) . . . . ?
N1' Rh1 C1B C2B 20.8(3) . . . . ?
C4B Rh1 C1B C2B 79.28(14) . . . . ?
C5B Rh1 C1B C2B 116.96(19) . . . . ?
C3B Rh1 C1B C2B 36.44(13) . . . . ?
Cl2 Rh1 C1B C2B -85.75(12) . . . . ?
C2 Rh1 C1B C6B -60.9(2) . . . . ?
N1' Rh1 C1B C6B 141.0(2) . . . . ?
C4B Rh1 C1B C6B -160.5(2) . . . . ?
C5B Rh1 C1B C6B -122.9(3) . . . . ?
C2B Rh1 C1B C6B 120.2(3) . . . . ?
C3B Rh1 C1B C6B 156.6(2) . . . . ?
Cl2 Rh1 C1B C6B 34.4(2) . . . . ?
C5B C1B C2B C3B 1.8(2) . . . . ?
C6B C1B C2B C3B 175.1(2) . . . . ?
Rh1 C1B C2B C3B -61.12(15) . . . . ?
C5B C1B C2B C7B -179.1(2) . . . . ?
C6B C1B C2B C7B -5.9(4) . . . . ?
Rh1 C1B C2B C7B 117.9(2) . . . . ?
C5B C1B C2B Rh1 62.96(15) . . . . ?
C6B C1B C2B Rh1 -123.8(2) . . . . ?
C2 Rh1 C2B C3B 115.9(2) . . . . ?
N1' Rh1 C2B C3B -53.25(16) . . . . ?
C4B Rh1 C2B C3B 36.88(13) . . . . ?
C1B Rh1 C2B C3B 118.15(19) . . . . ?
C5B Rh1 C2B C3B 80.42(15) . . . . ?
Cl2 Rh1 C2B C3B -143.83(13) . . . . ?
C2 Rh1 C2B C1B -2.2(3) . . . . ?
N1' Rh1 C2B C1B -171.41(12) . . . . ?
C4B Rh1 C2B C1B -81.28(14) . . . . ?
C5B Rh1 C2B C1B -37.73(13) . . . . ?
C3B Rh1 C2B C1B -118.2(2) . . . . ?
Cl2 Rh1 C2B C1B 98.01(12) . . . . ?
C2 Rh1 C2B C7B -121.7(2) . . . . ?
N1' Rh1 C2B C7B 69.1(2) . . . . ?
C4B Rh1 C2B C7B 159.2(2) . . . . ?
C1B Rh1 C2B C7B -119.5(2) . . . . ?
C5B Rh1 C2B C7B -157.2(2) . . . . ?
C3B Rh1 C2B C7B 122.4(3) . . . . ?
Cl2 Rh1 C2B C7B -21.48(19) . . . . ?
C1B C2B C3B C4B 0.8(2) . . . . ?
C7B C2B C3B C4B -178.2(2) . . . . ?
Rh1 C2B C3B C4B -58.38(15) . . . . ?
C1B C2B C3B C8B -179.7(2) . . . . ?
C7B C2B C3B C8B 1.2(4) . . . . ?
Rh1 C2B C3B C8B 121.1(2) . . . . ?
C1B C2B C3B Rh1 59.19(15) . . . . ?
C7B C2B C3B Rh1 -119.8(2) . . . . ?
C2 Rh1 C3B C2B -135.62(15) . . . . ?
N1' Rh1 C3B C2B 136.28(13) . . . . ?
C4B Rh1 C3B C2B -119.77(19) . . . . ?
C1B Rh1 C3B C2B -38.09(13) . . . . ?
C5B Rh1 C3B C2B -80.78(14) . . . . ?
Cl2 Rh1 C3B C2B 44.09(15) . . . . ?
C2 Rh1 C3B C4B -15.9(2) . . . . ?
N1' Rh1 C3B C4B -103.95(12) . . . . ?
C1B Rh1 C3B C4B 81.68(13) . . . . ?
C5B Rh1 C3B C4B 38.99(12) . . . . ?
C2B Rh1 C3B C4B 119.77(19) . . . . ?
Cl2 Rh1 C3B C4B 163.86(10) . . . . ?
C2 Rh1 C3B C8B 103.1(2) . . . . ?
N1' Rh1 C3B C8B 15.0(2) . . . . ?
C4B Rh1 C3B C8B 119.0(3) . . . . ?
C1B Rh1 C3B C8B -159.4(2) . . . . ?
C5B Rh1 C3B C8B 158.0(2) . . . . ?
C2B Rh1 C3B C8B -121.3(3) . . . . ?
Cl2 Rh1 C3B C8B -77.2(2) . . . . ?
C2B C3B C4B C5B -3.1(2) . . . . ?
C8B C3B C4B C5B 177.4(2) . . . . ?
Rh1 C3B C4B C5B -63.33(15) . . . . ?
C2B C3B C4B C9B -174.9(2) . . . . ?
C8B C3B C4B C9B 5.6(4) . . . . ?
Rh1 C3B C4B C9B 124.8(2) . . . . ?
C2B C3B C4B Rh1 60.23(15) . . . . ?
C8B C3B C4B Rh1 -119.2(2) . . . . ?
C2 Rh1 C4B C3B 170.81(12) . . . . ?
N1' Rh1 C4B C3B 82.51(13) . . . . ?
C1B Rh1 C4B C3B -79.05(14) . . . . ?
C5B Rh1 C4B C3B -115.94(19) . . . . ?
C2B Rh1 C4B C3B -35.71(12) . . . . ?
Cl2 Rh1 C4B C3B -37.5(2) . . . . ?
C2 Rh1 C4B C5B -73.25(14) . . . . ?
N1' Rh1 C4B C5B -161.55(13) . . . . ?
C1B Rh1 C4B C5B 36.89(13) . . . . ?
C2B Rh1 C4B C5B 80.23(14) . . . . ?
C3B Rh1 C4B C5B 115.94(19) . . . . ?
Cl2 Rh1 C4B C5B 78.4(2) . . . . ?
C2 Rh1 C4B C9B 48.1(2) . . . . ?
N1' Rh1 C4B C9B -40.2(2) . . . . ?
C1B Rh1 C4B C9B 158.3(2) . . . . ?
C5B Rh1 C4B C9B 121.4(3) . . . . ?
C2B Rh1 C4B C9B -158.4(2) . . . . ?
C3B Rh1 C4B C9B -122.7(3) . . . . ?
Cl2 Rh1 C4B C9B -160.22(15) . . . . ?
C2B C1B C5B C4B -3.7(2) . . . . ?
C6B C1B C5B C4B -176.7(2) . . . . ?
Rh1 C1B C5B C4B 60.01(15) . . . . ?
C2B C1B C5B C10B 174.7(2) . . . . ?
C6B C1B C5B C10B 1.7(4) . . . . ?
Rh1 C1B C5B C10B -121.5(2) . . . . ?
C2B C1B C5B Rh1 -63.74(15) . . . . ?
C6B C1B C5B Rh1 123.3(2) . . . . ?
C3B C4B C5B C1B 4.2(2) . . . . ?
C9B C4B C5B C1B 176.0(2) . . . . ?
Rh1 C4B C5B C1B -60.38(15) . . . . ?
C3B C4B C5B C10B -174.3(2) . . . . ?
C9B C4B C5B C10B -2.4(4) . . . . ?
Rh1 C4B C5B C10B 121.1(2) . . . . ?
C3B C4B C5B Rh1 64.60(15) . . . . ?
C9B C4B C5B Rh1 -123.6(2) . . . . ?
C2 Rh1 C5B C1B -126.99(14) . . . . ?
N1' Rh1 C5B C1B 146.64(14) . . . . ?
C4B Rh1 C5B C1B 118.5(2) . . . . ?
C2B Rh1 C5B C1B 38.47(13) . . . . ?
C3B Rh1 C5B C1B 80.03(15) . . . . ?
Cl2 Rh1 C5B C1B -30.95(17) . . . . ?
C2 Rh1 C5B C4B 114.53(14) . . . . ?
N1' Rh1 C5B C4B 28.16(19) . . . . ?
C1B Rh1 C5B C4B -118.5(2) . . . . ?
C2B Rh1 C5B C4B -80.01(14) . . . . ?
C3B Rh1 C5B C4B -38.45(13) . . . . ?
Cl2 Rh1 C5B C4B -149.43(11) . . . . ?
C2 Rh1 C5B C10B -5.2(2) . . . . ?
N1' Rh1 C5B C10B -91.6(2) . . . . ?
C4B Rh1 C5B C10B -119.7(3) . . . . ?
C1B Rh1 C5B C10B 121.8(3) . . . . ?
C2B Rh1 C5B C10B 160.2(2) . . . . ?
C3B Rh1 C5B C10B -158.2(2) . . . . ?
Cl2 Rh1 C5B C10B 90.8(2) . . . . ?
C21C B1C C11C C16C 17.2(3) . . . . ?
C36C B1C C11C C16C 136.70(19) . . . . ?
C41C B1C C11C C16C -103.9(2) . . . . ?
C21C B1C C11C C12C -166.36(18) . . . . ?
C36C B1C C11C C12C -46.8(2) . . . . ?
C41C B1C C11C C12C 72.6(2) . . . . ?
C16C C11C C12C C13C 2.8(3) . . . . ?
B1C C11C C12C C13C -174.01(19) . . . . ?
C11C C12C C13C C14C -1.4(3) . . . . ?
C12C C13C C14C C15C -0.7(3) . . . . ?
C13C C14C C15C C16C 1.2(3) . . . . ?
C14C C15C C16C C11C 0.3(3) . . . . ?
C12C C11C C16C C15C -2.2(3) . . . . ?
B1C C11C C16C C15C 174.45(18) . . . . ?
C11C B1C C21C C22C -82.3(2) . . . . ?
C36C B1C C21C C22C 157.14(19) . . . . ?
C41C B1C C21C C22C 37.8(3) . . . . ?
C11C B1C C21C C26C 92.5(2) . . . . ?
C36C B1C C21C C26C -28.0(3) . . . . ?
C41C B1C C21C C26C -147.36(19) . . . . ?
C26C C21C C22C C23C 0.9(3) . . . . ?
B1C C21C C22C C23C 176.1(2) . . . . ?
C21C C22C C23C C24C 0.1(3) . . . . ?
C22C C23C C24C C25C -1.4(3) . . . . ?
C23C C24C C25C C26C 1.5(3) . . . . ?
C24C C25C C26C C21C -0.4(3) . . . . ?
C22C C21C C26C C25C -0.8(3) . . . . ?
B1C C21C C26C C25C -175.9(2) . . . . ?
C36C C31C C32C C33C 0.4(4) . . . . ?
C31C C32C C33C C34C -0.3(3) . . . . ?
C32C C33C C34C C35C -0.3(3) . . . . ?
C33C C34C C35C C36C 0.8(3) . . . . ?
C34C C35C C36C C31C -0.7(3) . . . . ?
C34C C35C C36C B1C 176.08(18) . . . . ?
C32C C31C C36C C35C 0.1(3) . . . . ?
C32C C31C C36C B1C -176.7(2) . . . . ?
C11C B1C C36C C35C 151.77(17) . . . . ?
C21C B1C C36C C35C -89.2(2) . . . . ?
C41C B1C C36C C35C 31.7(2) . . . . ?
C11C B1C C36C C31C -31.7(2) . . . . ?
C21C B1C C36C C31C 87.3(2) . . . . ?
C41C B1C C36C C31C -151.78(19) . . . . ?
C11C B1C C41C C42C 155.68(18) . . . . ?
C21C B1C C41C C42C 36.3(3) . . . . ?
C36C B1C C41C C42C -83.5(2) . . . . ?
C11C B1C C41C C46C -28.9(3) . . . . ?
C21C B1C C41C C46C -148.3(2) . . . . ?
C36C B1C C41C C46C 91.9(2) . . . . ?
C46C C41C C42C C43C -0.5(3) . . . . ?
B1C C41C C42C C43C 175.3(2) . . . . ?
C41C C42C C43C C44C -0.1(3) . . . . ?
C42C C43C C44C C45C 0.4(3) . . . . ?
C43C C44C C45C C46C -0.3(4) . . . . ?
C44C C45C C46C C41C -0.3(4) . . . . ?
C42C C41C C46C C45C 0.7(3) . . . . ?
B1C C41C C46C C45C -175.0(2) . . . . ?
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max 0.320
_refine_diff_density_min -0.635
_refine_diff_density_rms 0.069
_iucr_refine_instructions_details
;
TITL Marina4 in P2(1)/n
CELL 0.71073 12.3833 24.7571 13.1128 90.000 92.980 90.000
ZERR 4.00 0.0009 0.0017 0.0009 0.000 0.002 0.000
LATT 1
SYMM 0.5-X, 0.5+Y, 0.5-Z
SFAC C H B N Cl Rh
UNIT 188 192 4 20 4 4
OMIT 0 2 0
OMIT 0 1 1
OMIT 1 1 0
OMIT 1 3 0
OMIT 0 2 1
OMIT -3 50
L.S. 15
ACTA
BOND $H
FMAP 2
PLAN 20
SIZE 0.279 0.247 0.087
CONF
TEMP -113.230
WGHT 0.041800 0.773100
FVAR 0.12391
MOLE 1
RH1 6 0.776096 0.925938 0.751331 11.00000 0.01992 0.01999 =
0.01782 -0.00062 0.00373 0.00028
CL2 5 0.807381 1.015238 0.819571 11.00000 0.03523 0.01880 =
0.02492 -0.00199 0.00357 -0.00022
N1 4 0.929792 0.894808 0.932872 11.00000 0.02218 0.02528 =
0.02792 0.00176 0.00056 0.00431
C2 1 0.831276 0.891568 0.883868 11.00000 0.02455 0.01893 =
0.02409 -0.00092 0.00470 0.00399
N3 4 0.775193 0.857018 0.941370 11.00000 0.02425 0.02205 =
0.02664 0.00616 0.00074 0.00242
C4 1 0.839267 0.838568 1.024278 11.00000 0.03507 0.02769 =
0.02786 0.01023 0.00188 0.00772
AFIX 43
H4 2 0.818625 0.813968 1.075346 11.00000 -1.20000
AFIX 0
C5 1 0.935223 0.862149 1.018034 11.00000 0.02863 0.03169 =
0.03095 0.00587 -0.00368 0.00926
AFIX 43
H5 2 0.996364 0.857341 1.063949 11.00000 -1.20000
AFIX 0
C6 1 1.015865 0.931735 0.906157 11.00000 0.02401 0.03203 =
0.04113 0.00489 0.00097 -0.00061
AFIX 137
H6A 2 1.070075 0.911953 0.869109 11.00000 -1.50000
H6B 2 1.049986 0.947254 0.968591 11.00000 -1.50000
H6C 2 0.985286 0.960774 0.862848 11.00000 -1.50000
AFIX 0
N1' 4 0.628443 0.925185 0.817882 11.00000 0.02277 0.02198 =
0.02136 0.00329 0.00342 0.00270
N2' 4 0.553953 0.962108 0.796065 11.00000 0.02204 0.02585 =
0.02490 0.00538 0.00659 0.00336
N3' 4 0.470252 0.948748 0.852571 11.00000 0.01926 0.02342 =
0.02552 0.00205 0.00497 -0.00065
C4' 1 0.491968 0.904615 0.910167 11.00000 0.02468 0.02353 =
0.02419 0.00329 0.00387 -0.00269
AFIX 43
H4' 2 0.446270 0.887783 0.956724 11.00000 -1.20000
AFIX 0
C5' 1 0.594132 0.889243 0.887130 11.00000 0.02261 0.02040 =
0.02283 0.00233 0.00202 -0.00179
C6' 1 0.373549 0.980652 0.842189 11.00000 0.02080 0.01915 =
0.02921 0.00037 0.00303 0.00045
C7' 1 0.341533 1.000694 0.747258 11.00000 0.02912 0.03189 =
0.02626 -0.00102 0.00370 0.00206
AFIX 43
H7' 2 0.382728 0.993451 0.689679 11.00000 -1.20000
AFIX 0
C8' 1 0.248477 1.031504 0.737294 11.00000 0.03342 0.02999 =
0.03357 0.00170 -0.00376 0.00462
AFIX 43
H8' 2 0.225708 1.045926 0.672567 11.00000 -1.20000
AFIX 0
C9' 1 0.188584 1.041352 0.821211 11.00000 0.02745 0.02825 =
0.04240 -0.00536 -0.00078 0.00592
AFIX 43
H9' 2 0.124360 1.062296 0.813990 11.00000 -1.20000
AFIX 0
C10' 1 0.221606 1.020947 0.915146 11.00000 0.02946 0.02873 =
0.03658 -0.00604 0.00840 0.00452
AFIX 43
H10' 2 0.179732 1.027807 0.972432 11.00000 -1.20000
AFIX 0
C11' 1 0.315192 0.990503 0.927335 11.00000 0.02939 0.02574 =
0.02658 -0.00030 0.00375 -0.00095
AFIX 43
H11' 2 0.338661 0.976761 0.992407 11.00000 -1.20000
AFIX 0
C1A 1 0.661287 0.841934 0.920774 11.00000 0.02636 0.02413 =
0.03229 0.00601 0.00245 -0.00171
AFIX 23
H1A1 2 0.632428 0.826450 0.983425 11.00000 -1.20000
H1A2 2 0.656541 0.813830 0.867021 11.00000 -1.20000
AFIX 0
C1B 1 0.890054 0.929544 0.633129 11.00000 0.03153 0.03651 =
0.01947 -0.00484 0.01208 -0.00418
C2B 1 0.789317 0.952932 0.591871 11.00000 0.04023 0.03605 =
0.01558 -0.00166 0.00535 -0.00367
C3B 1 0.709483 0.912362 0.593775 11.00000 0.03591 0.04256 =
0.01593 -0.00794 0.00183 -0.00295
C4B 1 0.757853 0.864226 0.636766 11.00000 0.03473 0.03084 =
0.02508 -0.01035 0.00678 -0.00269
C5B 1 0.871307 0.874785 0.656545 11.00000 0.03156 0.03276 =
0.02493 -0.01155 0.00950 0.00223
C6B 1 0.996948 0.958220 0.636852 11.00000 0.03798 0.05762 =
0.03527 -0.00254 0.01503 -0.01494
AFIX 137
H6B1 2 1.050727 0.936638 0.676274 11.00000 -1.50000
H6B2 2 0.989482 0.993546 0.669462 11.00000 -1.50000
H6B3 2 1.020443 0.963202 0.567253 11.00000 -1.50000
AFIX 0
C7B 1 0.773878 1.009755 0.556039 11.00000 0.06321 0.04208 =
0.02693 0.00854 0.00302 -0.00310
AFIX 137
H7B1 2 0.793534 1.012582 0.484800 11.00000 -1.50000
H7B2 2 0.819974 1.033858 0.598612 11.00000 -1.50000
H7B3 2 0.697989 1.020142 0.561174 11.00000 -1.50000
AFIX 0
C8B 1 0.593264 0.918434 0.557969 11.00000 0.03806 0.06668 =
0.03279 -0.01103 -0.00986 -0.00095
AFIX 137
H8B1 2 0.583750 0.906324 0.486917 11.00000 -1.50000
H8B2 2 0.572041 0.956454 0.562597 11.00000 -1.50000
H8B3 2 0.547969 0.896495 0.600969 11.00000 -1.50000
AFIX 0
C9B 1 0.703346 0.810397 0.645078 11.00000 0.04812 0.03609 =
0.04455 -0.01407 0.00741 -0.01048
AFIX 137
H9B1 2 0.628410 0.815742 0.663517 11.00000 -1.50000
H9B2 2 0.741942 0.788700 0.697791 11.00000 -1.50000
H9B3 2 0.704083 0.791590 0.579356 11.00000 -1.50000
AFIX 0
C10B 1 0.953813 0.834123 0.692681 11.00000 0.03889 0.04023 =
0.05169 -0.01534 0.00496 0.01225
AFIX 137
H10A 2 0.977853 0.813512 0.634220 11.00000 -1.50000
H10B 2 0.921884 0.809476 0.741246 11.00000 -1.50000
H10C 2 1.015829 0.852706 0.726284 11.00000 -1.50000
AFIX 0
MOLE 2
B1C 3 0.726765 0.251533 0.177971 11.00000 0.02412 0.01839 =
0.02211 -0.00031 -0.00278 0.00217
C11C 1 0.700701 0.213084 0.077449 11.00000 0.02182 0.02149 =
0.02064 -0.00002 0.00139 -0.00108
C12C 1 0.763252 0.167266 0.059228 11.00000 0.02268 0.02817 =
0.02955 -0.00132 -0.00505 0.00432
AFIX 43
H12C 2 0.816964 0.156807 0.109749 11.00000 -1.20000
AFIX 0
C13C 1 0.750662 0.136380 -0.028979 11.00000 0.02400 0.02473 =
0.03436 -0.00628 0.00456 0.00214
AFIX 43
H13C 2 0.796258 0.106113 -0.038327 11.00000 -1.20000
AFIX 0
C14C 1 0.671981 0.149645 -0.102990 11.00000 0.03066 0.02852 =
0.01966 -0.00389 0.00448 -0.00480
AFIX 43
H14C 2 0.663306 0.128997 -0.163931 11.00000 -1.20000
AFIX 0
C15C 1 0.605802 0.193608 -0.086926 11.00000 0.02753 0.02788 =
0.02269 0.00228 -0.00474 -0.00022
AFIX 43
H15C 2 0.550256 0.202878 -0.136539 11.00000 -1.20000
AFIX 0
C16C 1 0.620442 0.224165 0.001515 11.00000 0.02435 0.02056 =
0.02304 0.00153 -0.00016 0.00250
AFIX 43
H16C 2 0.573704 0.253993 0.010815 11.00000 -1.20000
AFIX 0
C21C 1 0.622494 0.291931 0.191114 11.00000 0.02519 0.02309 =
0.01864 -0.00727 -0.00621 0.00110
C22C 1 0.609463 0.339716 0.135303 11.00000 0.03012 0.02480 =
0.02714 -0.00296 -0.00483 0.00243
AFIX 43
H22C 2 0.664669 0.350201 0.091687 11.00000 -1.20000
AFIX 0
C23C 1 0.518757 0.372635 0.141006 11.00000 0.04043 0.02429 =
0.03662 -0.00438 -0.01533 0.00798
AFIX 43
H23C 2 0.512952 0.404809 0.101623 11.00000 -1.20000
AFIX 0
C24C 1 0.436973 0.358465 0.204116 11.00000 0.03072 0.03891 =
0.03949 -0.01751 -0.00948 0.01456
AFIX 43
H24C 2 0.375663 0.381161 0.209428 11.00000 -1.20000
AFIX 0
C25C 1 0.445569 0.311227 0.258904 11.00000 0.02807 0.04084 =
0.03396 -0.01261 0.00075 0.00462
AFIX 43
H25C 2 0.389180 0.300701 0.301144 11.00000 -1.20000
AFIX 0
C26C 1 0.536862 0.278721 0.252629 11.00000 0.02993 0.02960 =
0.02728 -0.00453 -0.00182 0.00337
AFIX 43
H26C 2 0.541326 0.246346 0.291511 11.00000 -1.20000
AFIX 0
C31C 1 0.692273 0.165310 0.295033 11.00000 0.03929 0.03058 =
0.02883 0.00231 -0.01208 -0.00672
AFIX 43
H31C 2 0.646545 0.152036 0.240243 11.00000 -1.20000
AFIX 0
C32C 1 0.702868 0.135019 0.383689 11.00000 0.04417 0.02677 =
0.03932 0.00650 -0.00439 -0.00959
AFIX 43
H32C 2 0.665231 0.101745 0.388357 11.00000 -1.20000
AFIX 0
C33C 1 0.768063 0.153043 0.465472 11.00000 0.03282 0.03133 =
0.02582 0.00844 0.00104 0.00536
AFIX 43
H33C 2 0.775487 0.132552 0.526689 11.00000 -1.20000
AFIX 0
C34C 1 0.821883 0.201167 0.456436 11.00000 0.02488 0.03555 =
0.02255 -0.00195 -0.00219 0.00364
AFIX 43
H34C 2 0.866773 0.214297 0.511950 11.00000 -1.20000
AFIX 0
C35C 1 0.810913 0.230803 0.366200 11.00000 0.02177 0.02216 =
0.02355 -0.00164 0.00198 0.00147
AFIX 43
H35C 2 0.849842 0.263712 0.361746 11.00000 -1.20000
AFIX 0
C36C 1 0.745401 0.214413 0.282012 11.00000 0.01837 0.02358 =
0.02312 -0.00205 0.00047 0.00447
C41C 1 0.838817 0.286805 0.161969 11.00000 0.02480 0.02678 =
0.02008 0.00619 -0.00604 0.00343
C42C 1 0.858414 0.335663 0.213126 11.00000 0.02641 0.02694 =
0.02627 0.00415 -0.00359 0.00126
AFIX 43
H42C 2 0.803724 0.349890 0.253648 11.00000 -1.20000
AFIX 0
C43C 1 0.954927 0.364481 0.207256 11.00000 0.03655 0.02824 =
0.03168 0.00704 -0.01106 -0.00346
AFIX 43
H43C 2 0.964879 0.397566 0.243225 11.00000 -1.20000
AFIX 0
C44C 1 1.035845 0.344649 0.148902 11.00000 0.02738 0.04695 =
0.03459 0.01618 -0.00596 -0.00855
AFIX 43
H44C 2 1.101950 0.363805 0.144799 11.00000 -1.20000
AFIX 0
C45C 1 1.019646 0.297058 0.097050 11.00000 0.02940 0.04692 =
0.03382 0.00506 0.00309 0.00101
AFIX 43
H45C 2 1.074732 0.283220 0.056541 11.00000 -1.20000
AFIX 0
C46C 1 0.923069 0.268867 0.103331 11.00000 0.03053 0.03463 =
0.02886 0.00098 -0.00020 0.00162
AFIX 43
H46C 2 0.913883 0.236069 0.066286 11.00000 -1.20000
HKLF 4
REM Marina4 in P2(1)/n
REM R1 = 0.0273 for 5955 Fo > 4sig(Fo) and 0.0353 for all 7047 data
REM 502 parameters refined using 0 restraints
END
WGHT 0.0411 0.8287
REM Highest difference peak 0.320, deepest hole -0.635, 1-sigma level 0.069
Q1 1 0.8158 0.8933 0.7679 11.00000 0.05 0.32
Q2 1 0.7095 0.2256 0.1253 11.00000 0.05 0.32
Q3 1 0.7140 0.1875 0.0758 11.00000 0.05 0.30
Q4 1 0.7400 0.1960 0.0562 11.00000 0.05 0.29
Q5 1 0.7430 0.1852 0.2787 11.00000 0.05 0.29
Q6 1 0.8423 0.2066 0.3982 11.00000 0.05 0.28
Q7 1 0.7163 0.1564 0.4383 11.00000 0.05 0.27
Q8 1 0.7355 0.2303 0.2295 11.00000 0.05 0.27
Q9 1 0.7758 0.1576 0.0005 11.00000 0.05 0.27
Q10 1 0.2789 0.2793 0.2516 11.00000 0.05 0.27
Q11 1 0.6823 0.1585 0.3509 11.00000 0.05 0.27
Q12 1 0.7269 0.8937 0.7444 11.00000 0.05 0.27
Q13 1 0.7946 0.1711 0.0688 11.00000 0.05 0.27
Q14 1 0.7819 0.1807 0.4546 11.00000 0.05 0.26
Q15 1 0.6613 0.1657 0.2780 11.00000 0.05 0.26
Q16 1 0.7118 0.1967 0.3007 11.00000 0.05 0.26
Q17 1 0.6589 0.1799 -0.1042 11.00000 0.05 0.26
Q18 1 0.3615 0.9974 0.8847 11.00000 0.05 0.26
Q19 1 0.6648 0.2162 0.0442 11.00000 0.05 0.25
Q20 1 0.7873 0.2165 0.4174 11.00000 0.05 0.24
;
_database_code_depnum_ccdc_archive 'CCDC 934045'
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_marina5_p1bar
#TrackingRef 'Marina5_Deposition_04Jul12.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C24 H30 Cl Ir N5, C24 H20 B, C H2 Cl2'
_chemical_formula_sum 'C49 H52 B Cl3 Ir N5'
_chemical_formula_weight 1020.32
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Triclinic
_symmetry_space_group_name_H-M 'P -1'
_symmetry_space_group_name_Hall '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 13.1491(5)
_cell_length_b 13.3892(5)
_cell_length_c 13.8083(5)
_cell_angle_alpha 67.1850(10)
_cell_angle_beta 87.363(2)
_cell_angle_gamma 88.838(2)
_cell_volume 2238.45(14)
_cell_formula_units_Z 2
_cell_measurement_temperature 160(2)
_cell_measurement_reflns_used 9862
_cell_measurement_theta_min 2.183
_cell_measurement_theta_max 30.452
_exptl_crystal_description Blocks
_exptl_crystal_colour 'Light yellow'
_exptl_crystal_size_max 0.23
_exptl_crystal_size_mid 0.23
_exptl_crystal_size_min 0.15
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.514
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1028
_exptl_absorpt_coefficient_mu 3.202
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.5276
_exptl_absorpt_correction_T_max 0.6452
_exptl_absorpt_process_details 'SADABS (Bruker, 2001)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 160(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker kappa APEXII CCD Diffractometer'
_diffrn_measurement_method '\f scans, and \w scans with \k offsets'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 49473
_diffrn_reflns_av_R_equivalents 0.0511
_diffrn_reflns_av_sigmaI/netI 0.0237
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_theta_min 2.26
_diffrn_reflns_theta_max 25.00
_reflns_number_total 7871
_reflns_number_gt 7458
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2007)'
_computing_cell_refinement 'APEX2 (Bruker, 2007)'
_computing_data_reduction 'APEX2 (Bruker, 2007)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+1.2757P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 7871
_refine_ls_number_parameters 538
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0222
_refine_ls_R_factor_gt 0.0204
_refine_ls_wR_factor_ref 0.0524
_refine_ls_wR_factor_gt 0.0518
_refine_ls_goodness_of_fit_ref 1.058
_refine_ls_restrained_S_all 1.058
_refine_ls_shift/su_max 0.004
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir1 Ir 0.741199(7) 0.880310(7) 0.710566(7) 0.01873(4) Uani 1 1 d . . .
Cl1 Cl 0.72548(5) 0.88434(5) 0.53364(5) 0.02429(13) Uani 1 1 d . . .
N1 N 0.82028(17) 0.65106(18) 0.74660(18) 0.0268(5) Uani 1 1 d . . .
C2 C 0.83607(19) 0.7511(2) 0.74434(19) 0.0215(5) Uani 1 1 d . . .
N3 N 0.93355(16) 0.74816(17) 0.77349(16) 0.0227(5) Uani 1 1 d . . .
C4 C 0.9775(2) 0.6474(2) 0.7940(2) 0.0295(6) Uani 1 1 d . . .
H4 H 1.0448 0.6257 0.8153 0.035 Uiso 1 1 calc R . .
C5 C 0.9060(2) 0.5873(2) 0.7778(2) 0.0330(7) Uani 1 1 d . . .
H5 H 0.9128 0.5136 0.7861 0.040 Uiso 1 1 calc R . .
C6 C 0.7271(2) 0.6120(3) 0.7192(3) 0.0371(7) Uani 1 1 d . . .
H6A H 0.6947 0.5579 0.7827 0.056 Uiso 1 1 calc R . .
H6B H 0.7440 0.5790 0.6683 0.056 Uiso 1 1 calc R . .
H6C H 0.6803 0.6729 0.6882 0.056 Uiso 1 1 calc R . .
C1A C 0.9843(2) 0.8394(2) 0.7841(2) 0.0262(6) Uani 1 1 d . . .
H1A1 H 1.0582 0.8242 0.7918 0.031 Uiso 1 1 calc R . .
H1A2 H 0.9569 0.8487 0.8481 0.031 Uiso 1 1 calc R . .
N1' N 0.87418(16) 0.97056(17) 0.65214(16) 0.0221(5) Uani 1 1 d . . .
N2' N 0.87754(16) 1.06526(18) 0.57205(17) 0.0247(5) Uani 1 1 d . . .
N3' N 0.97502(16) 1.09490(18) 0.55962(17) 0.0256(5) Uani 1 1 d . . .
C4' C 1.0340(2) 1.0215(2) 0.6298(2) 0.0270(6) Uani 1 1 d . . .
H4' H 1.1054 1.0247 0.6361 0.032 Uiso 1 1 calc R . .
C5' C 0.96835(19) 0.9408(2) 0.6905(2) 0.0225(5) Uani 1 1 d . . .
C6' C 1.0037(2) 1.2035(2) 0.4835(2) 0.0313(6) Uani 1 1 d . . .
H6'1 H 0.9527 1.2297 0.4285 0.038 Uiso 1 1 calc R . .
H6'2 H 1.0706 1.1998 0.4491 0.038 Uiso 1 1 calc R . .
C7' C 1.0096(2) 1.2814(2) 0.5377(2) 0.0330(7) Uani 1 1 d . . .
C8' C 0.9216(3) 1.3197(3) 0.5714(3) 0.0494(9) Uani 1 1 d . . .
H8' H 0.8568 1.2980 0.5588 0.059 Uiso 1 1 calc R . .
C9' C 0.9281(3) 1.3894(3) 0.6234(3) 0.0600(11) Uani 1 1 d . . .
H9' H 0.8678 1.4154 0.6465 0.072 Uiso 1 1 calc R . .
C10' C 1.0219(3) 1.4208(3) 0.6415(3) 0.0578(10) Uani 1 1 d . . .
H10' H 1.0261 1.4684 0.6772 0.069 Uiso 1 1 calc R . .
C11' C 1.1087(3) 1.3841(3) 0.6085(3) 0.0552(9) Uani 1 1 d . . .
H11' H 1.1733 1.4064 0.6209 0.066 Uiso 1 1 calc R . .
C12' C 1.1026(3) 1.3138(3) 0.5568(3) 0.0404(7) Uani 1 1 d . . .
H12' H 1.1633 1.2879 0.5343 0.048 Uiso 1 1 calc R . .
C1B C 0.66212(19) 0.8213(2) 0.8627(2) 0.0248(6) Uani 1 1 d . . .
C2B C 0.59130(19) 0.8319(2) 0.7839(2) 0.0255(6) Uani 1 1 d . . .
C3B C 0.58473(19) 0.9459(2) 0.7178(2) 0.0252(6) Uani 1 1 d . . .
C4B C 0.6534(2) 1.0031(2) 0.7509(2) 0.0275(6) Uani 1 1 d . . .
C5B C 0.70399(19) 0.9266(2) 0.8406(2) 0.0262(6) Uani 1 1 d . . .
C6B C 0.6870(2) 0.7193(3) 0.9536(2) 0.0363(7) Uani 1 1 d . . .
H6B1 H 0.6449 0.7148 1.0156 0.054 Uiso 1 1 calc R . .
H6B2 H 0.7591 0.7197 0.9687 0.054 Uiso 1 1 calc R . .
H6B3 H 0.6734 0.6567 0.9362 0.054 Uiso 1 1 calc R . .
C7B C 0.5213(2) 0.7470(3) 0.7797(3) 0.0359(7) Uani 1 1 d . . .
H7B1 H 0.5480 0.6750 0.8217 0.054 Uiso 1 1 calc R . .
H7B2 H 0.5164 0.7544 0.7066 0.054 Uiso 1 1 calc R . .
H7B3 H 0.4536 0.7560 0.8080 0.054 Uiso 1 1 calc R . .
C8B C 0.5133(2) 0.9923(3) 0.6296(2) 0.0395(7) Uani 1 1 d . . .
H8B1 H 0.4473 1.0071 0.6572 0.059 Uiso 1 1 calc R . .
H8B2 H 0.5043 0.9402 0.5967 0.059 Uiso 1 1 calc R . .
H8B3 H 0.5416 1.0597 0.5772 0.059 Uiso 1 1 calc R . .
C9B C 0.6706(3) 1.1228(3) 0.7063(3) 0.0421(8) Uani 1 1 d . . .
H9B1 H 0.6558 1.1528 0.6314 0.063 Uiso 1 1 calc R . .
H9B2 H 0.7416 1.1377 0.7146 0.063 Uiso 1 1 calc R . .
H9B3 H 0.6255 1.1565 0.7436 0.063 Uiso 1 1 calc R . .
C10B C 0.7759(2) 0.9566(3) 0.9065(2) 0.0372(7) Uani 1 1 d . . .
H10A H 0.8248 1.0103 0.8604 0.056 Uiso 1 1 calc R . .
H10B H 0.8126 0.8918 0.9511 0.056 Uiso 1 1 calc R . .
H10C H 0.7373 0.9873 0.9508 0.056 Uiso 1 1 calc R . .
B1C B 0.2482(2) 0.7565(3) 0.9595(3) 0.0279(7) Uani 1 1 d . . .
C11C C 0.2895(2) 0.8829(2) 0.9116(2) 0.0286(6) Uani 1 1 d . . .
C12C C 0.3873(2) 0.9118(2) 0.9276(2) 0.0314(6) Uani 1 1 d . . .
H12C H 0.4323 0.8563 0.9680 0.038 Uiso 1 1 calc R . .
C13C C 0.4212(2) 1.0190(3) 0.8865(2) 0.0381(7) Uani 1 1 d . . .
H13C H 0.4878 1.0352 0.8998 0.046 Uiso 1 1 calc R . .
C14C C 0.3583(3) 1.1014(3) 0.8267(2) 0.0431(8) Uani 1 1 d . . .
H14C H 0.3809 1.1744 0.7994 0.052 Uiso 1 1 calc R . .
C15C C 0.2620(3) 1.0763(3) 0.8070(2) 0.0427(8) Uani 1 1 d . . .
H15C H 0.2184 1.1321 0.7646 0.051 Uiso 1 1 calc R . .
C16C C 0.2291(2) 0.9702(3) 0.8490(2) 0.0365(7) Uani 1 1 d . . .
H16C H 0.1623 0.9551 0.8349 0.044 Uiso 1 1 calc R . .
C21C C 0.3209(2) 0.6843(2) 1.0570(2) 0.0307(6) Uani 1 1 d . . .
C22C C 0.4059(2) 0.6246(3) 1.0459(3) 0.0385(7) Uani 1 1 d . . .
H22C H 0.4189 0.6179 0.9805 0.046 Uiso 1 1 calc R . .
C23C C 0.4724(2) 0.5744(3) 1.1266(3) 0.0438(8) Uani 1 1 d . . .
H23C H 0.5293 0.5347 1.1153 0.053 Uiso 1 1 calc R . .
C24C C 0.4560(3) 0.5821(3) 1.2224(3) 0.0464(9) Uani 1 1 d . . .
H24C H 0.5017 0.5489 1.2772 0.056 Uiso 1 1 calc R . .
C25C C 0.3723(3) 0.6389(3) 1.2379(3) 0.0457(8) Uani 1 1 d . . .
H25C H 0.3597 0.6440 1.3042 0.055 Uiso 1 1 calc R . .
C26C C 0.3062(2) 0.6888(2) 1.1568(2) 0.0370(7) Uani 1 1 d . . .
H26C H 0.2491 0.7273 1.1693 0.044 Uiso 1 1 calc R . .
C31C C 0.25092(19) 0.7092(2) 0.8652(2) 0.0284(6) Uani 1 1 d . . .
C32C C 0.2503(2) 0.5974(3) 0.8869(3) 0.0344(7) Uani 1 1 d . . .
H32C H 0.2506 0.5478 0.9582 0.041 Uiso 1 1 calc R . .
C33C C 0.2493(2) 0.5564(3) 0.8089(3) 0.0419(8) Uani 1 1 d . . .
H33C H 0.2498 0.4802 0.8275 0.050 Uiso 1 1 calc R . .
C34C C 0.2476(2) 0.6255(3) 0.7043(3) 0.0457(8) Uani 1 1 d . . .
H34C H 0.2460 0.5975 0.6508 0.055 Uiso 1 1 calc R . .
C35C C 0.2483(2) 0.7361(3) 0.6787(3) 0.0403(8) Uani 1 1 d . . .
H35C H 0.2475 0.7847 0.6071 0.048 Uiso 1 1 calc R . .
C36C C 0.2502(2) 0.7761(3) 0.7579(2) 0.0319(6) Uani 1 1 d . . .
H36C H 0.2511 0.8524 0.7384 0.038 Uiso 1 1 calc R . .
C41C C 0.1297(2) 0.7509(2) 1.0076(2) 0.0274(6) Uani 1 1 d . . .
C42C C 0.0650(2) 0.6642(2) 1.0214(2) 0.0291(6) Uani 1 1 d . . .
H42C H 0.0893 0.6084 0.9999 0.035 Uiso 1 1 calc R . .
C43C C -0.0336(2) 0.6563(2) 1.0653(2) 0.0338(7) Uani 1 1 d . . .
H43C H -0.0749 0.5962 1.0724 0.041 Uiso 1 1 calc R . .
C44C C -0.0713(2) 0.7340(3) 1.0982(2) 0.0392(8) Uani 1 1 d . . .
H44C H -0.1384 0.7285 1.1283 0.047 Uiso 1 1 calc R . .
C45C C -0.0098(2) 0.8214(3) 1.0870(3) 0.0430(8) Uani 1 1 d . . .
H45C H -0.0348 0.8763 1.1094 0.052 Uiso 1 1 calc R . .
C46C C 0.0888(2) 0.8281(3) 1.0426(2) 0.0374(7) Uani 1 1 d . . .
H46C H 0.1297 0.8882 1.0361 0.045 Uiso 1 1 calc R . .
C1D C 0.5651(3) 0.7091(3) 0.4500(3) 0.0632(11) Uani 1 1 d . . .
H1D1 H 0.5423 0.7491 0.3777 0.076 Uiso 1 1 calc R . .
H1D2 H 0.6154 0.7548 0.4650 0.076 Uiso 1 1 calc R . .
Cl1D Cl 0.46071(8) 0.68627(8) 0.53891(7) 0.0599(2) Uani 1 1 d . . .
Cl2D Cl 0.62299(10) 0.58894(12) 0.45738(12) 0.0896(4) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ir1 0.01673(6) 0.02039(6) 0.01900(6) -0.00771(4) 0.00129(4) -0.00141(4)
Cl1 0.0229(3) 0.0321(3) 0.0207(3) -0.0135(3) 0.0015(2) -0.0027(3)
N1 0.0297(12) 0.0214(12) 0.0286(12) -0.0096(10) 0.0058(9) -0.0035(9)
C2 0.0219(13) 0.0213(13) 0.0198(13) -0.0068(11) 0.0060(10) -0.0034(10)
N3 0.0222(11) 0.0216(11) 0.0211(11) -0.0051(9) 0.0003(9) 0.0011(9)
C4 0.0322(15) 0.0249(15) 0.0267(14) -0.0053(12) 0.0007(11) 0.0078(12)
C5 0.0412(17) 0.0224(14) 0.0315(15) -0.0073(12) 0.0049(13) 0.0063(13)
C6 0.0373(17) 0.0309(16) 0.0474(18) -0.0200(14) 0.0035(14) -0.0099(13)
C1A 0.0227(13) 0.0261(15) 0.0272(14) -0.0074(12) -0.0014(11) -0.0020(11)
N1' 0.0219(11) 0.0219(12) 0.0218(11) -0.0081(9) 0.0020(9) -0.0018(9)
N2' 0.0263(12) 0.0220(12) 0.0230(11) -0.0059(10) 0.0028(9) -0.0042(9)
N3' 0.0258(12) 0.0214(12) 0.0272(12) -0.0072(10) 0.0047(9) -0.0064(9)
C4' 0.0216(13) 0.0280(15) 0.0309(15) -0.0112(12) 0.0019(11) -0.0058(11)
C5' 0.0212(13) 0.0226(14) 0.0239(13) -0.0093(11) 0.0009(10) -0.0038(10)
C6' 0.0371(16) 0.0233(14) 0.0258(14) -0.0020(12) 0.0094(12) -0.0076(12)
C7' 0.0452(18) 0.0215(14) 0.0261(15) -0.0034(12) 0.0098(13) -0.0034(13)
C8' 0.050(2) 0.0383(19) 0.055(2) -0.0150(17) 0.0178(17) -0.0034(15)
C9' 0.074(3) 0.044(2) 0.060(2) -0.0218(19) 0.028(2) 0.0070(19)
C10' 0.091(3) 0.041(2) 0.046(2) -0.0225(17) 0.015(2) -0.001(2)
C11' 0.065(2) 0.051(2) 0.059(2) -0.032(2) -0.0004(19) -0.0063(19)
C12' 0.0445(18) 0.0343(17) 0.0434(18) -0.0168(15) 0.0047(14) -0.0022(14)
C1B 0.0176(12) 0.0327(15) 0.0222(13) -0.0093(12) 0.0054(10) -0.0017(11)
C2B 0.0167(12) 0.0340(16) 0.0278(14) -0.0145(12) 0.0030(10) -0.0010(11)
C3B 0.0208(13) 0.0312(15) 0.0235(14) -0.0111(12) 0.0025(10) 0.0041(11)
C4B 0.0266(14) 0.0285(15) 0.0290(15) -0.0137(12) 0.0043(11) 0.0036(11)
C5B 0.0220(13) 0.0339(15) 0.0236(14) -0.0128(12) 0.0040(10) 0.0006(11)
C6B 0.0299(15) 0.0421(18) 0.0273(15) -0.0030(13) 0.0014(12) -0.0038(13)
C7B 0.0213(14) 0.0430(18) 0.0443(18) -0.0181(15) 0.0037(12) -0.0092(13)
C8B 0.0323(16) 0.049(2) 0.0366(17) -0.0160(15) -0.0075(13) 0.0104(14)
C9B 0.0476(19) 0.0320(17) 0.049(2) -0.0191(15) 0.0059(15) 0.0031(14)
C10B 0.0340(16) 0.052(2) 0.0378(17) -0.0302(16) 0.0007(13) -0.0066(14)
B1C 0.0213(15) 0.0310(17) 0.0301(17) -0.0101(14) -0.0027(12) -0.0006(13)
C11C 0.0295(14) 0.0319(16) 0.0261(14) -0.0134(12) -0.0001(11) 0.0012(12)
C12C 0.0279(15) 0.0366(17) 0.0301(15) -0.0138(13) 0.0046(12) -0.0013(12)
C13C 0.0352(16) 0.0420(19) 0.0396(17) -0.0193(15) 0.0123(13) -0.0115(14)
C14C 0.060(2) 0.0309(17) 0.0362(17) -0.0123(14) 0.0151(15) -0.0098(15)
C15C 0.058(2) 0.0347(18) 0.0327(17) -0.0102(14) -0.0014(15) 0.0070(15)
C16C 0.0381(17) 0.0378(18) 0.0352(16) -0.0159(14) -0.0053(13) 0.0044(13)
C21C 0.0240(14) 0.0256(15) 0.0383(16) -0.0071(13) -0.0049(12) -0.0058(11)
C22C 0.0249(15) 0.0382(18) 0.0409(18) -0.0030(14) 0.0041(13) -0.0022(13)
C23C 0.0236(15) 0.0314(17) 0.057(2) 0.0048(16) -0.0033(14) -0.0037(13)
C24C 0.0419(19) 0.0296(17) 0.056(2) -0.0009(16) -0.0250(16) -0.0071(14)
C25C 0.061(2) 0.0315(17) 0.0433(19) -0.0112(15) -0.0218(16) -0.0051(16)
C26C 0.0420(17) 0.0279(16) 0.0425(18) -0.0138(14) -0.0133(14) -0.0009(13)
C31C 0.0137(12) 0.0352(16) 0.0361(16) -0.0137(13) 0.0011(11) 0.0006(11)
C32C 0.0236(14) 0.0363(17) 0.0458(18) -0.0191(15) 0.0034(13) 0.0003(12)
C33C 0.0301(16) 0.0431(19) 0.060(2) -0.0293(17) 0.0072(14) -0.0015(14)
C34C 0.0336(17) 0.062(2) 0.057(2) -0.041(2) 0.0080(15) -0.0044(16)
C35C 0.0274(15) 0.060(2) 0.0381(18) -0.0237(16) 0.0035(13) -0.0042(14)
C36C 0.0196(13) 0.0392(17) 0.0387(17) -0.0176(14) 0.0014(11) 0.0003(12)
C41C 0.0221(13) 0.0347(16) 0.0232(14) -0.0085(12) -0.0064(11) 0.0027(11)
C42C 0.0277(14) 0.0299(15) 0.0249(14) -0.0054(12) -0.0034(11) 0.0053(12)
C43C 0.0286(15) 0.0342(17) 0.0292(15) -0.0018(13) -0.0028(12) -0.0035(12)
C44C 0.0246(15) 0.056(2) 0.0311(16) -0.0112(15) 0.0011(12) 0.0045(14)
C45C 0.0313(16) 0.059(2) 0.049(2) -0.0314(18) -0.0019(14) 0.0062(15)
C46C 0.0281(15) 0.0491(19) 0.0445(18) -0.0285(16) -0.0017(13) -0.0031(14)
C1D 0.062(2) 0.064(3) 0.059(2) -0.020(2) 0.0077(19) -0.004(2)
Cl1D 0.0685(6) 0.0570(6) 0.0475(5) -0.0137(4) 0.0056(4) 0.0028(5)
Cl2D 0.0696(7) 0.0970(10) 0.1256(11) -0.0700(9) 0.0049(7) 0.0068(7)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ir1 C2 2.026(3) . ?
Ir1 N1' 2.090(2) . ?
Ir1 C5B 2.149(3) . ?
Ir1 C1B 2.160(2) . ?
Ir1 C2B 2.165(3) . ?
Ir1 C4B 2.218(3) . ?
Ir1 C3B 2.234(3) . ?
Ir1 Cl1 2.4409(6) . ?
N1 C2 1.348(3) . ?
N1 C5 1.381(4) . ?
N1 C6 1.463(4) . ?
C2 N3 1.356(3) . ?
N3 C4 1.386(4) . ?
N3 C1A 1.464(3) . ?
C4 C5 1.331(4) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C1A C5' 1.486(4) . ?
C1A H1A1 0.9900 . ?
C1A H1A2 0.9900 . ?
N1' N2' 1.320(3) . ?
N1' C5' 1.360(3) . ?
N2' N3' 1.333(3) . ?
N3' C4' 1.344(4) . ?
N3' C6' 1.470(3) . ?
C4' C5' 1.372(4) . ?
C4' H4' 0.9500 . ?
C6' C7' 1.507(4) . ?
C6' H6'1 0.9900 . ?
C6' H6'2 0.9900 . ?
C7' C12' 1.375(4) . ?
C7' C8' 1.389(4) . ?
C8' C9' 1.386(5) . ?
C8' H8' 0.9500 . ?
C9' C10' 1.375(6) . ?
C9' H9' 0.9500 . ?
C10' C11' 1.362(5) . ?
C10' H10' 0.9500 . ?
C11' C12' 1.390(5) . ?
C11' H11' 0.9500 . ?
C12' H12' 0.9500 . ?
C1B C2B 1.429(4) . ?
C1B C5B 1.438(4) . ?
C1B C6B 1.496(4) . ?
C2B C3B 1.447(4) . ?
C2B C7B 1.497(4) . ?
C3B C4B 1.395(4) . ?
C3B C8B 1.499(4) . ?
C4B C5B 1.446(4) . ?
C4B C9B 1.496(4) . ?
C5B C10B 1.503(4) . ?
C6B H6B1 0.9800 . ?
C6B H6B2 0.9800 . ?
C6B H6B3 0.9800 . ?
C7B H7B1 0.9800 . ?
C7B H7B2 0.9800 . ?
C7B H7B3 0.9800 . ?
C8B H8B1 0.9800 . ?
C8B H8B2 0.9800 . ?
C8B H8B3 0.9800 . ?
C9B H9B1 0.9800 . ?
C9B H9B2 0.9800 . ?
C9B H9B3 0.9800 . ?
C10B H10A 0.9800 . ?
C10B H10B 0.9800 . ?
C10B H10C 0.9800 . ?
B1C C11C 1.654(4) . ?
B1C C21C 1.653(4) . ?
B1C C31C 1.653(4) . ?
B1C C41C 1.657(4) . ?
C11C C12C 1.402(4) . ?
C11C C16C 1.409(4) . ?
C12C C13C 1.397(4) . ?
C12C H12C 0.9500 . ?
C13C C14C 1.379(5) . ?
C13C H13C 0.9500 . ?
C14C C15C 1.383(5) . ?
C14C H14C 0.9500 . ?
C15C C16C 1.381(5) . ?
C15C H15C 0.9500 . ?
C16C H16C 0.9500 . ?
C21C C22C 1.397(4) . ?
C21C C26C 1.407(4) . ?
C22C C23C 1.395(4) . ?
C22C H22C 0.9500 . ?
C23C C24C 1.373(5) . ?
C23C H23C 0.9500 . ?
C24C C25C 1.381(5) . ?
C24C H24C 0.9500 . ?
C25C C26C 1.394(4) . ?
C25C H25C 0.9500 . ?
C26C H26C 0.9500 . ?
C31C C36C 1.402(4) . ?
C31C C32C 1.408(4) . ?
C32C C33C 1.387(4) . ?
C32C H32C 0.9500 . ?
C33C C34C 1.381(5) . ?
C33C H33C 0.9500 . ?
C34C C35C 1.383(5) . ?
C34C H34C 0.9500 . ?
C35C C36C 1.394(4) . ?
C35C H35C 0.9500 . ?
C36C H36C 0.9500 . ?
C41C C46C 1.391(4) . ?
C41C C42C 1.401(4) . ?
C42C C43C 1.395(4) . ?
C42C H42C 0.9500 . ?
C43C C44C 1.364(5) . ?
C43C H43C 0.9500 . ?
C44C C45C 1.390(5) . ?
C44C H44C 0.9500 . ?
C45C C46C 1.398(4) . ?
C45C H45C 0.9500 . ?
C46C H46C 0.9500 . ?
C1D Cl2D 1.735(4) . ?
C1D Cl1D 1.748(4) . ?
C1D H1D1 0.9900 . ?
C1D H1D2 0.9900 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Ir1 N1' 84.10(9) . . ?
C2 Ir1 C5B 114.58(10) . . ?
N1' Ir1 C5B 99.42(9) . . ?
C2 Ir1 C1B 95.08(10) . . ?
N1' Ir1 C1B 133.07(9) . . ?
C5B Ir1 C1B 38.98(10) . . ?
C2 Ir1 C2B 111.28(10) . . ?
N1' Ir1 C2B 161.27(10) . . ?
C5B Ir1 C2B 64.99(10) . . ?
C1B Ir1 C2B 38.58(10) . . ?
C2 Ir1 C4B 153.17(10) . . ?
N1' Ir1 C4B 97.66(9) . . ?
C5B Ir1 C4B 38.62(10) . . ?
C1B Ir1 C4B 64.18(10) . . ?
C2B Ir1 C4B 63.75(10) . . ?
C2 Ir1 C3B 149.29(10) . . ?
N1' Ir1 C3B 126.53(9) . . ?
C5B Ir1 C3B 63.27(10) . . ?
C1B Ir1 C3B 63.53(10) . . ?
C2B Ir1 C3B 38.36(10) . . ?
C4B Ir1 C3B 36.53(10) . . ?
C2 Ir1 Cl1 89.75(7) . . ?
N1' Ir1 Cl1 86.39(6) . . ?
C5B Ir1 Cl1 155.35(8) . . ?
C1B Ir1 Cl1 140.51(7) . . ?
C2B Ir1 Cl1 103.70(7) . . ?
C4B Ir1 Cl1 117.07(7) . . ?
C3B Ir1 Cl1 93.97(7) . . ?
C2 N1 C5 110.8(2) . . ?
C2 N1 C6 126.4(2) . . ?
C5 N1 C6 122.8(2) . . ?
N1 C2 N3 104.1(2) . . ?
N1 C2 Ir1 130.68(19) . . ?
N3 C2 Ir1 125.17(19) . . ?
C2 N3 C4 111.4(2) . . ?
C2 N3 C1A 123.9(2) . . ?
C4 N3 C1A 124.7(2) . . ?
C5 C4 N3 106.0(2) . . ?
C5 C4 H4 127.0 . . ?
N3 C4 H4 127.0 . . ?
C4 C5 N1 107.7(2) . . ?
C4 C5 H5 126.1 . . ?
N1 C5 H5 126.1 . . ?
N1 C6 H6A 109.5 . . ?
N1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N3 C1A C5' 110.6(2) . . ?
N3 C1A H1A1 109.5 . . ?
C5' C1A H1A1 109.5 . . ?
N3 C1A H1A2 109.5 . . ?
C5' C1A H1A2 109.5 . . ?
H1A1 C1A H1A2 108.1 . . ?
N2' N1' C5' 110.7(2) . . ?
N2' N1' Ir1 123.98(16) . . ?
C5' N1' Ir1 125.29(17) . . ?
N1' N2' N3' 105.2(2) . . ?
N2' N3' C4' 112.4(2) . . ?
N2' N3' C6' 119.3(2) . . ?
C4' N3' C6' 127.9(2) . . ?
N3' C4' C5' 104.8(2) . . ?
N3' C4' H4' 127.6 . . ?
C5' C4' H4' 127.6 . . ?
N1' C5' C4' 106.8(2) . . ?
N1' C5' C1A 121.3(2) . . ?
C4' C5' C1A 131.9(2) . . ?
N3' C6' C7' 110.5(2) . . ?
N3' C6' H6'1 109.5 . . ?
C7' C6' H6'1 109.5 . . ?
N3' C6' H6'2 109.5 . . ?
C7' C6' H6'2 109.5 . . ?
H6'1 C6' H6'2 108.1 . . ?
C12' C7' C8' 119.0(3) . . ?
C12' C7' C6' 120.3(3) . . ?
C8' C7' C6' 120.6(3) . . ?
C9' C8' C7' 120.1(4) . . ?
C9' C8' H8' 120.0 . . ?
C7' C8' H8' 120.0 . . ?
C10' C9' C8' 119.9(3) . . ?
C10' C9' H9' 120.0 . . ?
C8' C9' H9' 120.0 . . ?
C11' C10' C9' 120.5(4) . . ?
C11' C10' H10' 119.7 . . ?
C9' C10' H10' 119.7 . . ?
C10' C11' C12' 119.8(4) . . ?
C10' C11' H11' 120.1 . . ?
C12' C11' H11' 120.1 . . ?
C7' C12' C11' 120.7(3) . . ?
C7' C12' H12' 119.7 . . ?
C11' C12' H12' 119.7 . . ?
C2B C1B C5B 107.9(2) . . ?
C2B C1B C6B 126.3(3) . . ?
C5B C1B C6B 125.8(2) . . ?
C2B C1B Ir1 70.92(14) . . ?
C5B C1B Ir1 70.11(14) . . ?
C6B C1B Ir1 125.47(19) . . ?
C1B C2B C3B 107.2(2) . . ?
C1B C2B C7B 127.5(3) . . ?
C3B C2B C7B 124.4(2) . . ?
C1B C2B Ir1 70.50(14) . . ?
C3B C2B Ir1 73.39(15) . . ?
C7B C2B Ir1 129.96(19) . . ?
C4B C3B C2B 109.1(2) . . ?
C4B C3B C8B 126.9(3) . . ?
C2B C3B C8B 124.0(3) . . ?
C4B C3B Ir1 71.10(15) . . ?
C2B C3B Ir1 68.25(14) . . ?
C8B C3B Ir1 127.38(19) . . ?
C3B C4B C5B 108.1(2) . . ?
C3B C4B C9B 127.2(3) . . ?
C5B C4B C9B 124.6(3) . . ?
C3B C4B Ir1 72.37(15) . . ?
C5B C4B Ir1 68.13(15) . . ?
C9B C4B Ir1 126.9(2) . . ?
C1B C5B C4B 107.6(2) . . ?
C1B C5B C10B 127.0(3) . . ?
C4B C5B C10B 124.9(3) . . ?
C1B C5B Ir1 70.90(15) . . ?
C4B C5B Ir1 73.26(15) . . ?
C10B C5B Ir1 127.85(19) . . ?
C1B C6B H6B1 109.5 . . ?
C1B C6B H6B2 109.5 . . ?
H6B1 C6B H6B2 109.5 . . ?
C1B C6B H6B3 109.5 . . ?
H6B1 C6B H6B3 109.5 . . ?
H6B2 C6B H6B3 109.5 . . ?
C2B C7B H7B1 109.5 . . ?
C2B C7B H7B2 109.5 . . ?
H7B1 C7B H7B2 109.5 . . ?
C2B C7B H7B3 109.5 . . ?
H7B1 C7B H7B3 109.5 . . ?
H7B2 C7B H7B3 109.5 . . ?
C3B C8B H8B1 109.5 . . ?
C3B C8B H8B2 109.5 . . ?
H8B1 C8B H8B2 109.5 . . ?
C3B C8B H8B3 109.5 . . ?
H8B1 C8B H8B3 109.5 . . ?
H8B2 C8B H8B3 109.5 . . ?
C4B C9B H9B1 109.5 . . ?
C4B C9B H9B2 109.5 . . ?
H9B1 C9B H9B2 109.5 . . ?
C4B C9B H9B3 109.5 . . ?
H9B1 C9B H9B3 109.5 . . ?
H9B2 C9B H9B3 109.5 . . ?
C5B C10B H10A 109.5 . . ?
C5B C10B H10B 109.5 . . ?
H10A C10B H10B 109.5 . . ?
C5B C10B H10C 109.5 . . ?
H10A C10B H10C 109.5 . . ?
H10B C10B H10C 109.5 . . ?
C11C B1C C21C 108.1(2) . . ?
C11C B1C C31C 109.8(2) . . ?
C21C B1C C31C 111.9(2) . . ?
C11C B1C C41C 110.2(2) . . ?
C21C B1C C41C 108.1(2) . . ?
C31C B1C C41C 108.8(2) . . ?
C12C C11C C16C 114.8(3) . . ?
C12C C11C B1C 123.1(2) . . ?
C16C C11C B1C 122.1(2) . . ?
C13C C12C C11C 122.4(3) . . ?
C13C C12C H12C 118.8 . . ?
C11C C12C H12C 118.8 . . ?
C14C C13C C12C 120.3(3) . . ?
C14C C13C H13C 119.8 . . ?
C12C C13C H13C 119.8 . . ?
C13C C14C C15C 119.1(3) . . ?
C13C C14C H14C 120.4 . . ?
C15C C14C H14C 120.4 . . ?
C16C C15C C14C 119.9(3) . . ?
C16C C15C H15C 120.0 . . ?
C14C C15C H15C 120.0 . . ?
C15C C16C C11C 123.4(3) . . ?
C15C C16C H16C 118.3 . . ?
C11C C16C H16C 118.3 . . ?
C22C C21C C26C 114.9(3) . . ?
C22C C21C B1C 124.3(3) . . ?
C26C C21C B1C 120.5(3) . . ?
C23C C22C C21C 123.0(3) . . ?
C23C C22C H22C 118.5 . . ?
C21C C22C H22C 118.5 . . ?
C24C C23C C22C 120.1(3) . . ?
C24C C23C H23C 119.9 . . ?
C22C C23C H23C 119.9 . . ?
C23C C24C C25C 119.2(3) . . ?
C23C C24C H24C 120.4 . . ?
C25C C24C H24C 120.4 . . ?
C24C C25C C26C 120.2(3) . . ?
C24C C25C H25C 119.9 . . ?
C26C C25C H25C 119.9 . . ?
C25C C26C C21C 122.5(3) . . ?
C25C C26C H26C 118.7 . . ?
C21C C26C H26C 118.7 . . ?
C36C C31C C32C 114.6(3) . . ?
C36C C31C B1C 123.2(3) . . ?
C32C C31C B1C 122.1(3) . . ?
C33C C32C C31C 122.9(3) . . ?
C33C C32C H32C 118.6 . . ?
C31C C32C H32C 118.6 . . ?
C34C C33C C32C 120.5(3) . . ?
C34C C33C H33C 119.8 . . ?
C32C C33C H33C 119.8 . . ?
C33C C34C C35C 118.9(3) . . ?
C33C C34C H34C 120.5 . . ?
C35C C34C H34C 120.5 . . ?
C34C C35C C36C 120.0(3) . . ?
C34C C35C H35C 120.0 . . ?
C36C C35C H35C 120.0 . . ?
C35C C36C C31C 123.2(3) . . ?
C35C C36C H36C 118.4 . . ?
C31C C36C H36C 118.4 . . ?
C46C C41C C42C 114.9(3) . . ?
C46C C41C B1C 122.9(3) . . ?
C42C C41C B1C 122.1(3) . . ?
C43C C42C C41C 122.8(3) . . ?
C43C C42C H42C 118.6 . . ?
C41C C42C H42C 118.6 . . ?
C44C C43C C42C 120.5(3) . . ?
C44C C43C H43C 119.7 . . ?
C42C C43C H43C 119.7 . . ?
C43C C44C C45C 118.9(3) . . ?
C43C C44C H44C 120.5 . . ?
C45C C44C H44C 120.5 . . ?
C44C C45C C46C 119.8(3) . . ?
C44C C45C H45C 120.1 . . ?
C46C C45C H45C 120.1 . . ?
C41C C46C C45C 123.1(3) . . ?
C41C C46C H46C 118.5 . . ?
C45C C46C H46C 118.5 . . ?
Cl2D C1D Cl1D 111.9(2) . . ?
Cl2D C1D H1D1 109.2 . . ?
Cl1D C1D H1D1 109.2 . . ?
Cl2D C1D H1D2 109.2 . . ?
Cl1D C1D H1D2 109.2 . . ?
H1D1 C1D H1D2 107.9 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 C2 N3 0.7(3) . . . . ?
C6 N1 C2 N3 -178.5(2) . . . . ?
C5 N1 C2 Ir1 -177.75(19) . . . . ?
C6 N1 C2 Ir1 3.1(4) . . . . ?
N1' Ir1 C2 N1 -148.1(2) . . . . ?
C5B Ir1 C2 N1 114.2(2) . . . . ?
C1B Ir1 C2 N1 79.1(2) . . . . ?
C2B Ir1 C2 N1 42.9(3) . . . . ?
C4B Ir1 C2 N1 116.6(3) . . . . ?
C3B Ir1 C2 N1 35.7(4) . . . . ?
Cl1 Ir1 C2 N1 -61.7(2) . . . . ?
N1' Ir1 C2 N3 33.7(2) . . . . ?
C5B Ir1 C2 N3 -63.9(2) . . . . ?
C1B Ir1 C2 N3 -99.1(2) . . . . ?
C2B Ir1 C2 N3 -135.2(2) . . . . ?
C4B Ir1 C2 N3 -61.6(3) . . . . ?
C3B Ir1 C2 N3 -142.5(2) . . . . ?
Cl1 Ir1 C2 N3 120.1(2) . . . . ?
N1 C2 N3 C4 -0.2(3) . . . . ?
Ir1 C2 N3 C4 178.31(18) . . . . ?
N1 C2 N3 C1A -178.9(2) . . . . ?
Ir1 C2 N3 C1A -0.4(3) . . . . ?
C2 N3 C4 C5 -0.3(3) . . . . ?
C1A N3 C4 C5 178.4(2) . . . . ?
N3 C4 C5 N1 0.7(3) . . . . ?
C2 N1 C5 C4 -0.9(3) . . . . ?
C6 N1 C5 C4 178.3(2) . . . . ?
C2 N3 C1A C5' -47.8(3) . . . . ?
C4 N3 C1A C5' 133.7(3) . . . . ?
C2 Ir1 N1' N2' 147.8(2) . . . . ?
C5B Ir1 N1' N2' -98.1(2) . . . . ?
C1B Ir1 N1' N2' -120.7(2) . . . . ?
C2B Ir1 N1' N2' -65.9(4) . . . . ?
C4B Ir1 N1' N2' -59.1(2) . . . . ?
C3B Ir1 N1' N2' -34.5(2) . . . . ?
Cl1 Ir1 N1' N2' 57.73(19) . . . . ?
C2 Ir1 N1' C5' -32.2(2) . . . . ?
C5B Ir1 N1' C5' 81.8(2) . . . . ?
C1B Ir1 N1' C5' 59.2(2) . . . . ?
C2B Ir1 N1' C5' 114.1(3) . . . . ?
C4B Ir1 N1' C5' 120.8(2) . . . . ?
C3B Ir1 N1' C5' 145.4(2) . . . . ?
Cl1 Ir1 N1' C5' -122.3(2) . . . . ?
C5' N1' N2' N3' 0.4(3) . . . . ?
Ir1 N1' N2' N3' -179.64(16) . . . . ?
N1' N2' N3' C4' 0.0(3) . . . . ?
N1' N2' N3' C6' -173.3(2) . . . . ?
N2' N3' C4' C5' -0.4(3) . . . . ?
C6' N3' C4' C5' 172.2(2) . . . . ?
N2' N1' C5' C4' -0.6(3) . . . . ?
Ir1 N1' C5' C4' 179.41(17) . . . . ?
N2' N1' C5' C1A 177.2(2) . . . . ?
Ir1 N1' C5' C1A -2.7(3) . . . . ?
N3' C4' C5' N1' 0.6(3) . . . . ?
N3' C4' C5' C1A -177.0(3) . . . . ?
N3 C1A C5' N1' 48.2(3) . . . . ?
N3 C1A C5' C4' -134.5(3) . . . . ?
N2' N3' C6' C7' 95.5(3) . . . . ?
C4' N3' C6' C7' -76.5(4) . . . . ?
N3' C6' C7' C12' 104.7(3) . . . . ?
N3' C6' C7' C8' -73.8(4) . . . . ?
C12' C7' C8' C9' 0.0(5) . . . . ?
C6' C7' C8' C9' 178.5(3) . . . . ?
C7' C8' C9' C10' 0.1(6) . . . . ?
C8' C9' C10' C11' 0.1(6) . . . . ?
C9' C10' C11' C12' -0.4(6) . . . . ?
C8' C7' C12' C11' -0.3(5) . . . . ?
C6' C7' C12' C11' -178.7(3) . . . . ?
C10' C11' C12' C7' 0.4(5) . . . . ?
C2 Ir1 C1B C2B -118.23(17) . . . . ?
N1' Ir1 C1B C2B 155.10(15) . . . . ?
C5B Ir1 C1B C2B 118.1(2) . . . . ?
C4B Ir1 C1B C2B 79.56(17) . . . . ?
C3B Ir1 C1B C2B 38.69(16) . . . . ?
Cl1 Ir1 C1B C2B -22.4(2) . . . . ?
C2 Ir1 C1B C5B 123.65(16) . . . . ?
N1' Ir1 C1B C5B 37.0(2) . . . . ?
C2B Ir1 C1B C5B -118.1(2) . . . . ?
C4B Ir1 C1B C5B -38.57(15) . . . . ?
C3B Ir1 C1B C5B -79.43(16) . . . . ?
Cl1 Ir1 C1B C5B -140.56(13) . . . . ?
C2 Ir1 C1B C6B 3.2(3) . . . . ?
N1' Ir1 C1B C6B -83.4(3) . . . . ?
C5B Ir1 C1B C6B -120.4(3) . . . . ?
C2B Ir1 C1B C6B 121.5(3) . . . . ?
C4B Ir1 C1B C6B -159.0(3) . . . . ?
C3B Ir1 C1B C6B 160.2(3) . . . . ?
Cl1 Ir1 C1B C6B 99.0(2) . . . . ?
C5B C1B C2B C3B -4.1(3) . . . . ?
C6B C1B C2B C3B 174.7(2) . . . . ?
Ir1 C1B C2B C3B -64.74(17) . . . . ?
C5B C1B C2B C7B -173.4(3) . . . . ?
C6B C1B C2B C7B 5.4(4) . . . . ?
Ir1 C1B C2B C7B 126.0(3) . . . . ?
C5B C1B C2B Ir1 60.65(17) . . . . ?
C6B C1B C2B Ir1 -120.5(3) . . . . ?
C2 Ir1 C2B C1B 70.36(18) . . . . ?
N1' Ir1 C2B C1B -73.3(3) . . . . ?
C5B Ir1 C2B C1B -37.75(16) . . . . ?
C4B Ir1 C2B C1B -80.76(17) . . . . ?
C3B Ir1 C2B C1B -115.6(2) . . . . ?
Cl1 Ir1 C2B C1B 165.53(14) . . . . ?
C2 Ir1 C2B C3B -174.03(15) . . . . ?
N1' Ir1 C2B C3B 42.3(3) . . . . ?
C5B Ir1 C2B C3B 77.86(17) . . . . ?
C1B Ir1 C2B C3B 115.6(2) . . . . ?
C4B Ir1 C2B C3B 34.85(15) . . . . ?
Cl1 Ir1 C2B C3B -78.86(15) . . . . ?
C2 Ir1 C2B C7B -52.8(3) . . . . ?
N1' Ir1 C2B C7B 163.6(3) . . . . ?
C5B Ir1 C2B C7B -160.9(3) . . . . ?
C1B Ir1 C2B C7B -123.1(3) . . . . ?
C4B Ir1 C2B C7B 156.1(3) . . . . ?
C3B Ir1 C2B C7B 121.3(3) . . . . ?
Cl1 Ir1 C2B C7B 42.4(3) . . . . ?
C1B C2B C3B C4B 3.3(3) . . . . ?
C7B C2B C3B C4B 173.0(2) . . . . ?
Ir1 C2B C3B C4B -59.54(18) . . . . ?
C1B C2B C3B C8B -175.9(2) . . . . ?
C7B C2B C3B C8B -6.2(4) . . . . ?
Ir1 C2B C3B C8B 121.3(3) . . . . ?
C1B C2B C3B Ir1 62.83(17) . . . . ?
C7B C2B C3B Ir1 -127.4(3) . . . . ?
C2 Ir1 C3B C4B 131.5(2) . . . . ?
N1' Ir1 C3B C4B -43.83(19) . . . . ?
C5B Ir1 C3B C4B 37.83(16) . . . . ?
C1B Ir1 C3B C4B 81.66(17) . . . . ?
C2B Ir1 C3B C4B 120.6(2) . . . . ?
Cl1 Ir1 C3B C4B -132.28(15) . . . . ?
C2 Ir1 C3B C2B 10.9(3) . . . . ?
N1' Ir1 C3B C2B -164.40(14) . . . . ?
C5B Ir1 C3B C2B -82.73(17) . . . . ?
C1B Ir1 C3B C2B -38.91(15) . . . . ?
C4B Ir1 C3B C2B -120.6(2) . . . . ?
Cl1 Ir1 C3B C2B 107.16(14) . . . . ?
C2 Ir1 C3B C8B -106.0(3) . . . . ?
N1' Ir1 C3B C8B 78.7(3) . . . . ?
C5B Ir1 C3B C8B 160.3(3) . . . . ?
C1B Ir1 C3B C8B -155.8(3) . . . . ?
C2B Ir1 C3B C8B -116.9(3) . . . . ?
C4B Ir1 C3B C8B 122.5(3) . . . . ?
Cl1 Ir1 C3B C8B -9.8(3) . . . . ?
C2B C3B C4B C5B -1.2(3) . . . . ?
C8B C3B C4B C5B 178.0(3) . . . . ?
Ir1 C3B C4B C5B -58.98(17) . . . . ?
C2B C3B C4B C9B -178.8(3) . . . . ?
C8B C3B C4B C9B 0.3(5) . . . . ?
Ir1 C3B C4B C9B 123.4(3) . . . . ?
C2B C3B C4B Ir1 57.81(18) . . . . ?
C8B C3B C4B Ir1 -123.1(3) . . . . ?
C2 Ir1 C4B C3B -122.1(2) . . . . ?
N1' Ir1 C4B C3B 145.84(16) . . . . ?
C5B Ir1 C4B C3B -118.6(2) . . . . ?
C1B Ir1 C4B C3B -79.70(17) . . . . ?
C2B Ir1 C4B C3B -36.57(16) . . . . ?
Cl1 Ir1 C4B C3B 55.99(17) . . . . ?
C2 Ir1 C4B C5B -3.5(3) . . . . ?
N1' Ir1 C4B C5B -95.53(16) . . . . ?
C1B Ir1 C4B C5B 38.93(15) . . . . ?
C2B Ir1 C4B C5B 82.06(17) . . . . ?
C3B Ir1 C4B C5B 118.6(2) . . . . ?
Cl1 Ir1 C4B C5B 174.62(13) . . . . ?
C2 Ir1 C4B C9B 114.2(3) . . . . ?
N1' Ir1 C4B C9B 22.2(3) . . . . ?
C5B Ir1 C4B C9B 117.7(3) . . . . ?
C1B Ir1 C4B C9B 156.6(3) . . . . ?
C2B Ir1 C4B C9B -160.2(3) . . . . ?
C3B Ir1 C4B C9B -123.7(3) . . . . ?
Cl1 Ir1 C4B C9B -67.7(3) . . . . ?
C2B C1B C5B C4B 3.4(3) . . . . ?
C6B C1B C5B C4B -175.4(2) . . . . ?
Ir1 C1B C5B C4B 64.57(17) . . . . ?
C2B C1B C5B C10B 175.3(3) . . . . ?
C6B C1B C5B C10B -3.5(4) . . . . ?
Ir1 C1B C5B C10B -123.5(3) . . . . ?
C2B C1B C5B Ir1 -61.17(17) . . . . ?
C6B C1B C5B Ir1 120.0(3) . . . . ?
C3B C4B C5B C1B -1.4(3) . . . . ?
C9B C4B C5B C1B 176.4(3) . . . . ?
Ir1 C4B C5B C1B -63.03(17) . . . . ?
C3B C4B C5B C10B -173.5(2) . . . . ?
C9B C4B C5B C10B 4.2(4) . . . . ?
Ir1 C4B C5B C10B 124.8(3) . . . . ?
C3B C4B C5B Ir1 61.65(18) . . . . ?
C9B C4B C5B Ir1 -120.6(3) . . . . ?
C2 Ir1 C5B C1B -65.76(17) . . . . ?
N1' Ir1 C5B C1B -153.55(15) . . . . ?
C2B Ir1 C5B C1B 37.36(15) . . . . ?
C4B Ir1 C5B C1B 116.0(2) . . . . ?
C3B Ir1 C5B C1B 80.15(16) . . . . ?
Cl1 Ir1 C5B C1B 104.4(2) . . . . ?
C2 Ir1 C5B C4B 178.29(15) . . . . ?
N1' Ir1 C5B C4B 90.50(16) . . . . ?
C1B Ir1 C5B C4B -116.0(2) . . . . ?
C2B Ir1 C5B C4B -78.59(17) . . . . ?
C3B Ir1 C5B C4B -35.80(15) . . . . ?
Cl1 Ir1 C5B C4B -11.5(3) . . . . ?
C2 Ir1 C5B C10B 56.8(3) . . . . ?
N1' Ir1 C5B C10B -31.0(3) . . . . ?
C1B Ir1 C5B C10B 122.5(3) . . . . ?
C2B Ir1 C5B C10B 159.9(3) . . . . ?
C4B Ir1 C5B C10B -121.5(3) . . . . ?
C3B Ir1 C5B C10B -157.3(3) . . . . ?
Cl1 Ir1 C5B C10B -133.1(2) . . . . ?
C21C B1C C11C C12C 19.6(4) . . . . ?
C31C B1C C11C C12C -102.7(3) . . . . ?
C41C B1C C11C C12C 137.5(3) . . . . ?
C21C B1C C11C C16C -162.0(3) . . . . ?
C31C B1C C11C C16C 75.7(3) . . . . ?
C41C B1C C11C C16C -44.1(4) . . . . ?
C16C C11C C12C C13C 1.3(4) . . . . ?
B1C C11C C12C C13C 179.9(3) . . . . ?
C11C C12C C13C C14C -0.7(4) . . . . ?
C12C C13C C14C C15C -0.8(5) . . . . ?
C13C C14C C15C C16C 1.4(5) . . . . ?
C14C C15C C16C C11C -0.7(5) . . . . ?
C12C C11C C16C C15C -0.7(4) . . . . ?
B1C C11C C16C C15C -179.2(3) . . . . ?
C11C B1C C21C C22C -94.6(3) . . . . ?
C31C B1C C21C C22C 26.3(4) . . . . ?
C41C B1C C21C C22C 146.1(3) . . . . ?
C11C B1C C21C C26C 78.6(3) . . . . ?
C31C B1C C21C C26C -160.4(2) . . . . ?
C41C B1C C21C C26C -40.6(3) . . . . ?
C26C C21C C22C C23C -1.0(4) . . . . ?
B1C C21C C22C C23C 172.6(3) . . . . ?
C21C C22C C23C C24C 0.1(5) . . . . ?
C22C C23C C24C C25C 0.9(5) . . . . ?
C23C C24C C25C C26C -0.9(5) . . . . ?
C24C C25C C26C C21C -0.1(5) . . . . ?
C22C C21C C26C C25C 1.0(4) . . . . ?
B1C C21C C26C C25C -172.9(3) . . . . ?
C11C B1C C31C C36C -22.1(3) . . . . ?
C21C B1C C31C C36C -142.1(3) . . . . ?
C41C B1C C31C C36C 98.6(3) . . . . ?
C11C B1C C31C C32C 160.3(2) . . . . ?
C21C B1C C31C C32C 40.3(3) . . . . ?
C41C B1C C31C C32C -79.0(3) . . . . ?
C36C C31C C32C C33C 0.1(4) . . . . ?
B1C C31C C32C C33C 177.9(3) . . . . ?
C31C C32C C33C C34C -0.8(4) . . . . ?
C32C C33C C34C C35C 0.8(5) . . . . ?
C33C C34C C35C C36C -0.3(5) . . . . ?
C34C C35C C36C C31C -0.4(4) . . . . ?
C32C C31C C36C C35C 0.5(4) . . . . ?
B1C C31C C36C C35C -177.3(2) . . . . ?
C11C B1C C41C C46C -24.8(4) . . . . ?
C21C B1C C41C C46C 93.1(3) . . . . ?
C31C B1C C41C C46C -145.2(3) . . . . ?
C11C B1C C41C C42C 158.8(2) . . . . ?
C21C B1C C41C C42C -83.3(3) . . . . ?
C31C B1C C41C C42C 38.4(3) . . . . ?
C46C C41C C42C C43C 1.0(4) . . . . ?
B1C C41C C42C C43C 177.6(3) . . . . ?
C41C C42C C43C C44C -0.6(4) . . . . ?
C42C C43C C44C C45C 0.1(4) . . . . ?
C43C C44C C45C C46C 0.0(5) . . . . ?
C42C C41C C46C C45C -0.8(4) . . . . ?
B1C C41C C46C C45C -177.4(3) . . . . ?
C44C C45C C46C C41C 0.4(5) . . . . ?
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max 0.909
_refine_diff_density_min -0.833
_refine_diff_density_rms 0.084
_iucr_refine_instructions_details
;
TITL Marina5_P1bar in P-1
CELL 0.71073 13.1491 13.3892 13.8083 67.185 87.363 88.838
ZERR 2.00 0.0005 0.0005 0.0005 0.001 0.002 0.002
LATT 1
SFAC C H B N Cl Ir
UNIT 98 104 2 10 6 2
OMIT 0 1 1
OMIT 0 1 0
OMIT 1 0 0
OMIT 0 2 0
OMIT 0 0 1
OMIT -1 0 1
OMIT 1 0 1
OMIT 1 2 1
OMIT -1 1 0
OMIT 1 1 1
OMIT 0 -1 1
OMIT -1 1 1
OMIT -3 50
L.S. 15
ACTA
BOND $H
FMAP 2
PLAN 20
CONF
SIZE 0.229 0.228 0.150
TEMP -112.950
WGHT 0.031300 1.275700
FVAR 0.17469
MOLE 1
IR1 6 0.741199 0.880310 0.710566 11.00000 0.01673 0.02039 =
0.01900 -0.00771 0.00129 -0.00141
CL1 5 0.725478 0.884340 0.533638 11.00000 0.02290 0.03212 =
0.02069 -0.01347 0.00145 -0.00270
N1 4 0.820284 0.651063 0.746604 11.00000 0.02968 0.02143 =
0.02858 -0.00964 0.00576 -0.00355
C2 1 0.836072 0.751128 0.744343 11.00000 0.02191 0.02132 =
0.01978 -0.00677 0.00604 -0.00340
N3 4 0.933552 0.748157 0.773491 11.00000 0.02223 0.02157 =
0.02112 -0.00506 0.00029 0.00106
C4 1 0.977458 0.647426 0.793975 11.00000 0.03220 0.02489 =
0.02665 -0.00531 0.00068 0.00784
AFIX 43
H4 2 1.044817 0.625739 0.815254 11.00000 -1.20000
AFIX 0
C5 1 0.906048 0.587255 0.777768 11.00000 0.04120 0.02237 =
0.03149 -0.00728 0.00491 0.00634
AFIX 43
H5 2 0.912843 0.513617 0.786134 11.00000 -1.20000
AFIX 0
C6 1 0.727112 0.611982 0.719166 11.00000 0.03728 0.03085 =
0.04744 -0.02005 0.00350 -0.00987
AFIX 137
H6A 2 0.694680 0.557926 0.782661 11.00000 -1.50000
H6B 2 0.743956 0.578957 0.668303 11.00000 -1.50000
H6C 2 0.680294 0.672885 0.688156 11.00000 -1.50000
AFIX 0
C1A 1 0.984337 0.839444 0.784091 11.00000 0.02272 0.02611 =
0.02717 -0.00743 -0.00138 -0.00202
AFIX 23
H1A1 2 1.058167 0.824187 0.791804 11.00000 -1.20000
H1A2 2 0.956943 0.848736 0.848081 11.00000 -1.20000
AFIX 0
N1' 4 0.874181 0.970564 0.652140 11.00000 0.02192 0.02185 =
0.02184 -0.00805 0.00203 -0.00179
N2' 4 0.877543 1.065255 0.572046 11.00000 0.02633 0.02196 =
0.02296 -0.00594 0.00277 -0.00415
N3' 4 0.975018 1.094900 0.559618 11.00000 0.02575 0.02144 =
0.02720 -0.00722 0.00474 -0.00639
C4' 1 1.033975 1.021451 0.629843 11.00000 0.02160 0.02805 =
0.03094 -0.01115 0.00187 -0.00576
AFIX 43
H4' 2 1.105370 1.024669 0.636069 11.00000 -1.20000
AFIX 0
C5' 1 0.968352 0.940833 0.690532 11.00000 0.02119 0.02258 =
0.02386 -0.00927 0.00088 -0.00376
C6' 1 1.003697 1.203472 0.483548 11.00000 0.03713 0.02330 =
0.02579 -0.00199 0.00943 -0.00762
AFIX 23
H6'1 2 0.952720 1.229713 0.428535 11.00000 -1.20000
H6'2 2 1.070565 1.199804 0.449063 11.00000 -1.20000
AFIX 0
C7' 1 1.009625 1.281427 0.537748 11.00000 0.04519 0.02154 =
0.02612 -0.00345 0.00984 -0.00343
C8' 1 0.921555 1.319652 0.571435 11.00000 0.04954 0.03831 =
0.05548 -0.01495 0.01785 -0.00339
AFIX 43
H8' 2 0.856782 1.297998 0.558835 11.00000 -1.20000
AFIX 0
C9' 1 0.928087 1.389355 0.623414 11.00000 0.07392 0.04369 =
0.06049 -0.02185 0.02765 0.00698
AFIX 43
H9' 2 0.867847 1.415385 0.646523 11.00000 -1.20000
AFIX 0
C10' 1 1.021869 1.420757 0.641472 11.00000 0.09055 0.04066 =
0.04571 -0.02255 0.01519 -0.00128
AFIX 43
H10' 2 1.026125 1.468438 0.677209 11.00000 -1.20000
AFIX 0
C11' 1 1.108730 1.384061 0.608543 11.00000 0.06502 0.05093 =
0.05903 -0.03155 -0.00037 -0.00629
AFIX 43
H11' 2 1.173282 1.406410 0.620917 11.00000 -1.20000
AFIX 0
C12' 1 1.102611 1.313812 0.556777 11.00000 0.04454 0.03434 =
0.04340 -0.01680 0.00473 -0.00218
AFIX 43
H12' 2 1.163282 1.287901 0.534310 11.00000 -1.20000
AFIX 0
C1B 1 0.662121 0.821264 0.862725 11.00000 0.01760 0.03274 =
0.02217 -0.00928 0.00545 -0.00175
C2B 1 0.591302 0.831871 0.783861 11.00000 0.01666 0.03401 =
0.02783 -0.01448 0.00300 -0.00097
C3B 1 0.584728 0.945929 0.717808 11.00000 0.02085 0.03121 =
0.02354 -0.01106 0.00253 0.00409
C4B 1 0.653398 1.003052 0.750942 11.00000 0.02656 0.02847 =
0.02903 -0.01374 0.00434 0.00361
C5B 1 0.703988 0.926592 0.840641 11.00000 0.02203 0.03388 =
0.02356 -0.01282 0.00402 0.00064
C6B 1 0.687024 0.719332 0.953629 11.00000 0.02989 0.04211 =
0.02727 -0.00297 0.00139 -0.00384
AFIX 137
H6B1 2 0.644857 0.714807 1.015581 11.00000 -1.50000
H6B2 2 0.759089 0.719714 0.968698 11.00000 -1.50000
H6B3 2 0.673445 0.656682 0.936177 11.00000 -1.50000
AFIX 0
C7B 1 0.521274 0.746972 0.779697 11.00000 0.02129 0.04296 =
0.04429 -0.01806 0.00370 -0.00919
AFIX 137
H7B1 2 0.547974 0.674981 0.821733 11.00000 -1.50000
H7B2 2 0.516443 0.754370 0.706612 11.00000 -1.50000
H7B3 2 0.453565 0.755989 0.808019 11.00000 -1.50000
AFIX 0
C8B 1 0.513288 0.992258 0.629564 11.00000 0.03226 0.04906 =
0.03662 -0.01596 -0.00748 0.01040
AFIX 137
H8B1 2 0.447257 1.007148 0.657173 11.00000 -1.50000
H8B2 2 0.504323 0.940166 0.596681 11.00000 -1.50000
H8B3 2 0.541583 1.059746 0.577154 11.00000 -1.50000
AFIX 0
C9B 1 0.670573 1.122820 0.706278 11.00000 0.04761 0.03196 =
0.04900 -0.01906 0.00594 0.00314
AFIX 137
H9B1 2 0.655840 1.152781 0.631429 11.00000 -1.50000
H9B2 2 0.741620 1.137661 0.714577 11.00000 -1.50000
H9B3 2 0.625510 1.156479 0.743569 11.00000 -1.50000
AFIX 0
C10B 1 0.775925 0.956606 0.906461 11.00000 0.03395 0.05154 =
0.03780 -0.03016 0.00069 -0.00660
AFIX 137
H10A 2 0.824813 1.010253 0.860412 11.00000 -1.50000
H10B 2 0.812551 0.891787 0.951078 11.00000 -1.50000
H10C 2 0.737306 0.987344 0.950798 11.00000 -1.50000
AFIX 0
MOLE 2
B1C 3 0.248205 0.756473 0.959465 11.00000 0.02127 0.03097 =
0.03006 -0.01013 -0.00266 -0.00059
C11C 1 0.289507 0.882949 0.911614 11.00000 0.02955 0.03193 =
0.02612 -0.01336 -0.00012 0.00122
C12C 1 0.387315 0.911759 0.927649 11.00000 0.02788 0.03656 =
0.03010 -0.01383 0.00463 -0.00127
AFIX 43
H12C 2 0.432267 0.856324 0.967997 11.00000 -1.20000
AFIX 0
C13C 1 0.421158 1.019001 0.886485 11.00000 0.03524 0.04195 =
0.03958 -0.01931 0.01229 -0.01150
AFIX 43
H13C 2 0.487813 1.035225 0.899777 11.00000 -1.20000
AFIX 0
C14C 1 0.358319 1.101398 0.826678 11.00000 0.06030 0.03091 =
0.03621 -0.01228 0.01510 -0.00981
AFIX 43
H14C 2 0.380932 1.174439 0.799368 11.00000 -1.20000
AFIX 0
C15C 1 0.261951 1.076327 0.806968 11.00000 0.05769 0.03468 =
0.03269 -0.01025 -0.00138 0.00697
AFIX 43
H15C 2 0.218409 1.132096 0.764581 11.00000 -1.20000
AFIX 0
C16C 1 0.229080 0.970155 0.848959 11.00000 0.03809 0.03784 =
0.03519 -0.01589 -0.00525 0.00438
AFIX 43
H16C 2 0.162298 0.955131 0.834886 11.00000 -1.20000
AFIX 0
C21C 1 0.320948 0.684330 1.056970 11.00000 0.02396 0.02558 =
0.03826 -0.00710 -0.00493 -0.00581
C22C 1 0.405870 0.624611 1.045938 11.00000 0.02486 0.03817 =
0.04089 -0.00297 0.00411 -0.00218
AFIX 43
H22C 2 0.418863 0.617923 0.980465 11.00000 -1.20000
AFIX 0
C23C 1 0.472443 0.574366 1.126645 11.00000 0.02362 0.03135 =
0.05687 0.00482 -0.00329 -0.00371
AFIX 43
H23C 2 0.529263 0.534675 1.115338 11.00000 -1.20000
AFIX 0
C24C 1 0.456046 0.582137 1.222373 11.00000 0.04190 0.02962 =
0.05610 -0.00093 -0.02503 -0.00707
AFIX 43
H24C 2 0.501730 0.548880 1.277238 11.00000 -1.20000
AFIX 0
C25C 1 0.372306 0.638906 1.237931 11.00000 0.06133 0.03154 =
0.04331 -0.01122 -0.02177 -0.00514
AFIX 43
H25C 2 0.359695 0.643955 1.304182 11.00000 -1.20000
AFIX 0
C26C 1 0.306234 0.688814 1.156773 11.00000 0.04198 0.02792 =
0.04252 -0.01379 -0.01329 -0.00095
AFIX 43
H26C 2 0.249076 0.727334 1.169324 11.00000 -1.20000
AFIX 0
C31C 1 0.250917 0.709187 0.865152 11.00000 0.01372 0.03518 =
0.03607 -0.01368 0.00113 0.00063
C32C 1 0.250323 0.597370 0.886938 11.00000 0.02359 0.03626 =
0.04580 -0.01905 0.00342 0.00031
AFIX 43
H32C 2 0.250642 0.547850 0.958215 11.00000 -1.20000
AFIX 0
C33C 1 0.249291 0.556371 0.808867 11.00000 0.03013 0.04312 =
0.06001 -0.02928 0.00721 -0.00146
AFIX 43
H33C 2 0.249754 0.480217 0.827464 11.00000 -1.20000
AFIX 0
C34C 1 0.247596 0.625460 0.704302 11.00000 0.03360 0.06171 =
0.05726 -0.04097 0.00805 -0.00442
AFIX 43
H34C 2 0.245974 0.597462 0.650833 11.00000 -1.20000
AFIX 0
C35C 1 0.248297 0.736072 0.678702 11.00000 0.02736 0.05967 =
0.03808 -0.02371 0.00350 -0.00415
AFIX 43
H35C 2 0.247480 0.784748 0.607144 11.00000 -1.20000
AFIX 0
C36C 1 0.250202 0.776101 0.757933 11.00000 0.01964 0.03922 =
0.03871 -0.01759 0.00136 0.00027
AFIX 43
H36C 2 0.251058 0.852384 0.738368 11.00000 -1.20000
AFIX 0
C41C 1 0.129737 0.750881 1.007582 11.00000 0.02209 0.03474 =
0.02317 -0.00849 -0.00639 0.00273
C42C 1 0.065005 0.664188 1.021370 11.00000 0.02769 0.02985 =
0.02495 -0.00545 -0.00342 0.00534
AFIX 43
H42C 2 0.089339 0.608381 0.999866 11.00000 -1.20000
AFIX 0
C43C 1 -0.033635 0.656275 1.065310 11.00000 0.02859 0.03420 =
0.02920 -0.00181 -0.00275 -0.00352
AFIX 43
H43C 2 -0.074935 0.596236 1.072396 11.00000 -1.20000
AFIX 0
C44C 1 -0.071281 0.734013 1.098184 11.00000 0.02462 0.05609 =
0.03111 -0.01119 0.00114 0.00453
AFIX 43
H44C 2 -0.138421 0.728544 1.128258 11.00000 -1.20000
AFIX 0
C45C 1 -0.009829 0.821386 1.086978 11.00000 0.03127 0.05863 =
0.04862 -0.03137 -0.00186 0.00621
AFIX 43
H45C 2 -0.034759 0.876349 1.109402 11.00000 -1.20000
AFIX 0
C46C 1 0.088763 0.828097 1.042608 11.00000 0.02814 0.04909 =
0.04451 -0.02846 -0.00174 -0.00309
AFIX 43
H46C 2 0.129707 0.888209 1.036065 11.00000 -1.20000
AFIX 0
MOLE 3
C1D 1 0.565116 0.709118 0.449985 11.00000 0.06202 0.06419 =
0.05868 -0.01972 0.00770 -0.00361
AFIX 23
H1D1 2 0.542255 0.749084 0.377688 11.00000 -1.20000
H1D2 2 0.615374 0.754762 0.464974 11.00000 -1.20000
AFIX 0
CL1D 5 0.460706 0.686271 0.538907 11.00000 0.06847 0.05697 =
0.04749 -0.01370 0.00559 0.00284
CL2D 5 0.622993 0.588941 0.457381 11.00000 0.06958 0.09701 =
0.12564 -0.07005 0.00486 0.00677
HKLF 4
REM Marina5_P1bar in P-1
REM R1 = 0.0204 for 7458 Fo > 4sig(Fo) and 0.0222 for all 7871 data
REM 538 parameters refined using 0 restraints
END
WGHT 0.0305 1.3347
REM Highest difference peak 0.909, deepest hole -0.833, 1-sigma level 0.084
Q1 1 0.8008 0.8508 0.6935 11.00000 0.05 0.91
Q2 1 0.6981 0.8385 0.6950 11.00000 0.05 0.79
Q3 1 0.6808 0.9130 0.7116 11.00000 0.05 0.76
Q4 1 0.7565 0.8626 0.5427 11.00000 0.05 0.59
Q5 1 0.7220 0.8622 0.5197 11.00000 0.05 0.50
Q6 1 0.7201 0.9142 0.4989 11.00000 0.05 0.49
Q7 1 0.7826 0.7816 0.7496 11.00000 0.05 0.39
Q8 1 0.5247 0.6591 0.5166 11.00000 0.05 0.38
Q9 1 0.5830 0.6324 0.3836 11.00000 0.05 0.36
Q10 1 0.8533 0.6121 0.7729 11.00000 0.05 0.32
Q11 1 0.9802 0.8849 0.7394 11.00000 0.05 0.30
Q12 1 0.9620 0.6997 0.7895 11.00000 0.05 0.30
Q13 1 0.8821 1.2448 0.5068 11.00000 0.05 0.30
Q14 1 0.9596 0.7929 0.7782 11.00000 0.05 0.29
Q15 1 0.8640 1.1645 0.5421 11.00000 0.05 0.28
Q16 1 0.6798 0.6307 0.3986 11.00000 0.05 0.27
Q17 1 0.2540 0.9192 0.8861 11.00000 0.05 0.27
Q18 1 0.8728 0.8023 0.7105 11.00000 0.05 0.27
Q19 1 0.8201 0.9552 0.6612 11.00000 0.05 0.27
Q20 1 0.6210 0.9647 0.7249 11.00000 0.05 0.27
;
_database_code_depnum_ccdc_archive 'CCDC 934046'
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_marina7_p21byc
#TrackingRef 'Marina7_Deposition_04Jul12.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety '2(C31 H36 Cl N5 Rh), 2(C24 H20 B), C H2 Cl2'
_chemical_formula_sum 'C111 H114 B2 Cl4 N10 Rh2 '
_chemical_formula_weight 1957.36
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M 'P 21/c'
_symmetry_space_group_name_Hall '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 15.2978(8)
_cell_length_b 12.1192(7)
_cell_length_c 26.5776(14)
_cell_angle_alpha 90.00
_cell_angle_beta 96.241(2)
_cell_angle_gamma 90.00
_cell_volume 4898.2(5)
_cell_formula_units_Z 2
_cell_measurement_temperature 150(2)
_cell_measurement_reflns_used 9813
_cell_measurement_theta_min 2.149
_cell_measurement_theta_max 30.267
_exptl_crystal_description Plates
_exptl_crystal_colour 'Dark orange'
_exptl_crystal_size_max 0.28
_exptl_crystal_size_mid 0.19
_exptl_crystal_size_min 0.10
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.327
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 2036.0
_exptl_absorpt_coefficient_mu 0.500
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.8882
_exptl_absorpt_correction_T_max 0.9594
_exptl_absorpt_process_details 'SADABS (Bruker, 2001)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 150(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker kappa APEXII CCD Diffractometer'
_diffrn_measurement_method '\f scans, and \w scans with \k offsets'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 49243
_diffrn_reflns_av_R_equivalents 0.0264
_diffrn_reflns_av_sigmaI/netI 0.0212
_diffrn_reflns_limit_h_min -18
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_l_min -31
_diffrn_reflns_limit_l_max 27
_diffrn_reflns_theta_min 2.33
_diffrn_reflns_theta_max 25.00
_reflns_number_total 8609
_reflns_number_gt 7228
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2007)'
_computing_cell_refinement 'APEX2 (Bruker, 2007)'
_computing_data_reduction 'APEX2 (Bruker, 2007)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1175P)^2^+15.1912P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 8609
_refine_ls_number_parameters 603
_refine_ls_number_restraints 4
_refine_ls_R_factor_all 0.0784
_refine_ls_R_factor_gt 0.0670
_refine_ls_wR_factor_ref 0.2028
_refine_ls_wR_factor_gt 0.1898
_refine_ls_goodness_of_fit_ref 1.037
_refine_ls_restrained_S_all 1.037
_refine_ls_shift/su_max 0.009
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1D C 0.5267(10) 0.4066(13) 0.1892(8) 0.180(11) Uani 0.50 1 d PDU . .
H1D1 H 0.4842 0.4618 0.1739 0.216 Uiso 0.50 1 calc PR . .
H1D2 H 0.5401 0.4246 0.2255 0.216 Uiso 0.50 1 calc PR . .
Cl1D Cl 0.4794(3) 0.2748(6) 0.18301(17) 0.1117(16) Uani 0.50 1 d PDU . .
Cl2D Cl 0.6234(3) 0.4137(5) 0.15969(19) 0.1050(14) Uani 0.50 1 d PDU . .
Rh1 Rh 0.72590(2) 0.19038(4) 0.362478(12) 0.03873(17) Uani 1 1 d . . .
Cl1 Cl 0.57599(8) 0.20966(17) 0.32511(4) 0.0655(5) Uani 1 1 d . . .
N1 N 0.6915(3) 0.4376(4) 0.3939(2) 0.0574(13) Uani 1 1 d . . .
C2 C 0.7184(4) 0.3339(5) 0.4038(2) 0.0476(13) Uani 1 1 d . . .
N3 N 0.7363(3) 0.3329(4) 0.45550(18) 0.0499(12) Uani 1 1 d . . .
C4 C 0.7223(4) 0.4319(6) 0.4776(3) 0.0611(16) Uani 1 1 d . . .
H4 H 0.7315 0.4497 0.5125 0.073 Uiso 1 1 calc R . .
C5 C 0.6934(4) 0.4972(6) 0.4400(3) 0.0680(19) Uani 1 1 d . . .
H5 H 0.6765 0.5721 0.4432 0.082 Uiso 1 1 calc R . .
C6 C 0.6802(5) 0.4957(6) 0.3466(3) 0.077(2) Uani 1 1 d . . .
C7 C 0.6010(5) 0.5225(7) 0.3264(3) 0.075(2) Uani 1 1 d . . .
C8 C 0.5959(5) 0.5926(8) 0.2841(3) 0.091(3) Uani 1 1 d . . .
H8 H 0.5396 0.6131 0.2682 0.109 Uiso 1 1 calc R . .
C9 C 0.6708(5) 0.6331(8) 0.2648(3) 0.086(2) Uani 1 1 d . . .
C10 C 0.7517(5) 0.6080(7) 0.2903(3) 0.078(2) Uani 1 1 d . . .
H10 H 0.8025 0.6386 0.2780 0.093 Uiso 1 1 calc R . .
C11 C 0.7631(5) 0.5427(6) 0.3315(2) 0.0662(17) Uani 1 1 d . . .
C12 C 0.5143(5) 0.4798(9) 0.3467(3) 0.105(4) Uani 1 1 d . . .
H12A H 0.5268 0.4588 0.3824 0.158 Uiso 1 1 calc R . .
H12B H 0.4921 0.4155 0.3269 0.158 Uiso 1 1 calc R . .
H12C H 0.4699 0.5384 0.3435 0.158 Uiso 1 1 calc R . .
C13 C 0.6625(6) 0.7101(8) 0.2199(4) 0.098(3) Uani 1 1 d . . .
H13A H 0.7202 0.7422 0.2158 0.146 Uiso 1 1 calc R . .
H13B H 0.6209 0.7692 0.2254 0.146 Uiso 1 1 calc R . .
H13C H 0.6412 0.6690 0.1893 0.146 Uiso 1 1 calc R . .
C14 C 0.8483(5) 0.5186(7) 0.3598(3) 0.078(2) Uani 1 1 d . . .
H14A H 0.8513 0.5527 0.3934 0.117 Uiso 1 1 calc R . .
H14B H 0.8954 0.5483 0.3415 0.117 Uiso 1 1 calc R . .
H14C H 0.8555 0.4385 0.3635 0.117 Uiso 1 1 calc R . .
C1A C 0.7696(4) 0.2383(5) 0.48500(18) 0.0508(14) Uani 1 1 d . . .
H1A1 H 0.7745 0.2569 0.5215 0.061 Uiso 1 1 calc R . .
H1A2 H 0.8291 0.2193 0.4762 0.061 Uiso 1 1 calc R . .
N1' N 0.6808(2) 0.1138(4) 0.42736(14) 0.0384(10) Uani 1 1 d . . .
N2' N 0.6337(3) 0.0236(4) 0.42694(15) 0.0432(10) Uani 1 1 d . . .
N3' N 0.6335(3) -0.0046(4) 0.47602(15) 0.0424(10) Uani 1 1 d . . .
C4' C 0.6802(3) 0.0675(5) 0.50646(18) 0.0467(13) Uani 1 1 d . . .
H4' H 0.6898 0.0659 0.5424 0.056 Uiso 1 1 calc R . .
C5' C 0.7107(3) 0.1431(5) 0.47500(17) 0.0421(12) Uani 1 1 d . . .
C6' C 0.5886(3) -0.1026(5) 0.4889(2) 0.0491(13) Uani 1 1 d . . .
C7' C 0.5677(5) -0.1814(6) 0.4534(3) 0.0662(18) Uani 1 1 d . . .
H7' H 0.5828 -0.1724 0.4199 0.079 Uiso 1 1 calc R . .
C8' C 0.5235(6) -0.2765(7) 0.4669(3) 0.084(2) Uani 1 1 d . . .
H8' H 0.5079 -0.3318 0.4422 0.100 Uiso 1 1 calc R . .
C9' C 0.5023(5) -0.2908(6) 0.5155(3) 0.075(2) Uani 1 1 d . . .
H9' H 0.4715 -0.3549 0.5241 0.090 Uiso 1 1 calc R . .
C10' C 0.5259(5) -0.2120(6) 0.5513(3) 0.072(2) Uani 1 1 d . . .
H10' H 0.5137 -0.2231 0.5853 0.086 Uiso 1 1 calc R . .
C11' C 0.5678(4) -0.1151(6) 0.5383(2) 0.0618(16) Uani 1 1 d . . .
H11' H 0.5819 -0.0589 0.5627 0.074 Uiso 1 1 calc R . .
C1B C 0.8655(3) 0.1929(5) 0.35135(19) 0.0447(13) Uani 1 1 d . . .
C2B C 0.8120(4) 0.2143(5) 0.30383(19) 0.0496(14) Uani 1 1 d . . .
C3B C 0.7616(3) 0.1171(6) 0.29132(17) 0.0519(15) Uani 1 1 d . . .
C4B C 0.7767(3) 0.0397(5) 0.33084(18) 0.0470(13) Uani 1 1 d . . .
C5B C 0.8415(3) 0.0888(5) 0.36792(17) 0.0410(12) Uani 1 1 d . . .
C6B C 0.9399(4) 0.2573(7) 0.3762(2) 0.0649(17) Uani 1 1 d . . .
H6B1 H 0.9940 0.2136 0.3773 0.097 Uiso 1 1 calc R . .
H6B2 H 0.9285 0.2757 0.4108 0.097 Uiso 1 1 calc R . .
H6B3 H 0.9467 0.3254 0.3572 0.097 Uiso 1 1 calc R . .
C7B C 0.8196(5) 0.3086(6) 0.2682(2) 0.069(2) Uani 1 1 d . . .
H7B1 H 0.7607 0.3352 0.2558 0.104 Uiso 1 1 calc R . .
H7B2 H 0.8498 0.2838 0.2395 0.104 Uiso 1 1 calc R . .
H7B3 H 0.8532 0.3684 0.2859 0.104 Uiso 1 1 calc R . .
C8B C 0.7030(5) 0.1023(8) 0.2430(2) 0.084(3) Uani 1 1 d . . .
H8B1 H 0.6632 0.0400 0.2464 0.126 Uiso 1 1 calc R . .
H8B2 H 0.7389 0.0875 0.2154 0.126 Uiso 1 1 calc R . .
H8B3 H 0.6685 0.1696 0.2355 0.126 Uiso 1 1 calc R . .
C9B C 0.7383(4) -0.0730(6) 0.3320(3) 0.0658(17) Uani 1 1 d . . .
H9B1 H 0.7748 -0.1247 0.3150 0.099 Uiso 1 1 calc R . .
H9B2 H 0.6786 -0.0725 0.3144 0.099 Uiso 1 1 calc R . .
H9B3 H 0.7365 -0.0960 0.3672 0.099 Uiso 1 1 calc R . .
C10B C 0.8812(4) 0.0323(6) 0.4151(2) 0.0578(16) Uani 1 1 d . . .
H10A H 0.9038 0.0877 0.4400 0.087 Uiso 1 1 calc R . .
H10B H 0.9295 -0.0154 0.4070 0.087 Uiso 1 1 calc R . .
H10C H 0.8363 -0.0125 0.4291 0.087 Uiso 1 1 calc R . .
B1C B 0.0695(4) 0.7518(5) 0.88291(19) 0.0355(12) Uani 1 1 d . . .
C11C C 0.0203(3) 0.7481(4) 0.82415(16) 0.0323(10) Uani 1 1 d . . .
C12C C 0.0160(3) 0.8388(4) 0.79124(17) 0.0367(10) Uani 1 1 d . . .
H12D H 0.0453 0.9049 0.8025 0.044 Uiso 1 1 calc R . .
C13C C -0.0292(3) 0.8366(5) 0.74274(19) 0.0429(12) Uani 1 1 d . . .
H13D H -0.0301 0.9001 0.7217 0.052 Uiso 1 1 calc R . .
C14C C -0.0731(3) 0.7410(5) 0.72520(18) 0.0447(12) Uani 1 1 d . . .
H14D H -0.1048 0.7387 0.6924 0.054 Uiso 1 1 calc R . .
C15C C -0.0698(3) 0.6500(5) 0.75633(19) 0.0439(12) Uani 1 1 d . . .
H15C H -0.0994 0.5843 0.7449 0.053 Uiso 1 1 calc R . .
C16C C -0.0238(3) 0.6530(4) 0.80422(18) 0.0378(11) Uani 1 1 d . . .
H16C H -0.0219 0.5882 0.8244 0.045 Uiso 1 1 calc R . .
C21C C 0.1084(3) 0.6274(4) 0.89761(16) 0.0344(10) Uani 1 1 d . . .
C22C C 0.1573(4) 0.5671(5) 0.86487(19) 0.0482(13) Uani 1 1 d . . .
H22C H 0.1704 0.6017 0.8345 0.058 Uiso 1 1 calc R . .
C23C C 0.1872(4) 0.4607(5) 0.8744(2) 0.0504(13) Uani 1 1 d . . .
H23C H 0.2205 0.4245 0.8512 0.060 Uiso 1 1 calc R . .
C24C C 0.1684(4) 0.4071(4) 0.9181(2) 0.0464(12) Uani 1 1 d . . .
H24C H 0.1881 0.3337 0.9250 0.056 Uiso 1 1 calc R . .
C25C C 0.1207(3) 0.4621(4) 0.95117(18) 0.0410(11) Uani 1 1 d . . .
H25C H 0.1070 0.4263 0.9811 0.049 Uiso 1 1 calc R . .
C26C C 0.0922(3) 0.5694(4) 0.94120(16) 0.0340(10) Uani 1 1 d . . .
H26C H 0.0602 0.6054 0.9651 0.041 Uiso 1 1 calc R . .
C31C C 0.1486(3) 0.8446(4) 0.88660(16) 0.0375(11) Uani 1 1 d . . .
C32C C 0.2370(4) 0.8202(5) 0.88657(18) 0.0473(13) Uani 1 1 d . . .
H32C H 0.2541 0.7449 0.8858 0.057 Uiso 1 1 calc R . .
C33C C 0.3027(4) 0.9012(6) 0.8876(2) 0.0603(17) Uani 1 1 d . . .
H33C H 0.3625 0.8801 0.8875 0.072 Uiso 1 1 calc R . .
C34C C 0.2804(5) 1.0115(6) 0.8889(2) 0.067(2) Uani 1 1 d . . .
H34C H 0.3243 1.0671 0.8898 0.080 Uiso 1 1 calc R . .
C35C C 0.1928(5) 1.0391(5) 0.8886(2) 0.0597(17) Uani 1 1 d . . .
H35C H 0.1764 1.1147 0.8890 0.072 Uiso 1 1 calc R . .
C36C C 0.1281(4) 0.9580(4) 0.88786(18) 0.0469(13) Uani 1 1 d . . .
H36C H 0.0685 0.9797 0.8882 0.056 Uiso 1 1 calc R . .
C41C C -0.0038(4) 0.7828(4) 0.92178(18) 0.0385(11) Uani 1 1 d . . .
C42C C 0.0162(4) 0.8411(4) 0.96669(18) 0.0427(12) Uani 1 1 d . . .
H42C H 0.0744 0.8677 0.9749 0.051 Uiso 1 1 calc R . .
C43C C -0.0471(4) 0.8621(5) 1.00046(19) 0.0495(14) Uani 1 1 d . . .
H43C H -0.0313 0.9035 1.0304 0.059 Uiso 1 1 calc R . .
C44C C -0.1307(5) 0.8230(5) 0.9902(2) 0.0569(16) Uani 1 1 d . . .
H44C H -0.1731 0.8365 1.0131 0.068 Uiso 1 1 calc R . .
C45C C -0.1533(4) 0.7641(6) 0.9465(2) 0.0618(16) Uani 1 1 d . . .
H45C H -0.2112 0.7356 0.9393 0.074 Uiso 1 1 calc R . .
C46C C -0.0907(4) 0.7463(5) 0.9129(2) 0.0504(13) Uani 1 1 d . . .
H46C H -0.1081 0.7073 0.8824 0.061 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1D 0.040(8) 0.249(14) 0.25(3) -0.21(2) 0.031(10) -0.014(11)
Cl1D 0.079(3) 0.188(5) 0.066(2) -0.004(3) -0.006(2) 0.023(3)
Cl2D 0.068(2) 0.145(4) 0.102(3) -0.023(3) 0.009(2) 0.033(2)
Rh1 0.0290(2) 0.0715(3) 0.0165(2) 0.00216(16) 0.00595(15) 0.01176(17)
Cl1 0.0214(6) 0.1574(16) 0.0168(5) 0.0019(7) -0.0023(4) 0.0329(7)
N1 0.049(3) 0.067(3) 0.061(3) 0.010(3) 0.029(2) 0.004(2)
C2 0.046(3) 0.065(4) 0.036(3) 0.004(2) 0.023(2) 0.001(3)
N3 0.046(3) 0.067(3) 0.041(2) -0.014(2) 0.022(2) -0.009(2)
C4 0.061(4) 0.067(4) 0.060(4) -0.009(3) 0.025(3) -0.006(3)
C5 0.055(4) 0.066(4) 0.087(5) -0.024(4) 0.027(3) 0.001(3)
C6 0.078(5) 0.078(5) 0.084(5) 0.037(4) 0.047(4) 0.039(4)
C7 0.063(4) 0.109(6) 0.054(4) 0.025(4) 0.009(3) 0.009(4)
C8 0.053(4) 0.118(7) 0.099(6) 0.030(5) 0.003(4) 0.014(4)
C9 0.061(4) 0.119(7) 0.077(5) 0.037(5) 0.007(4) 0.004(4)
C10 0.067(4) 0.083(5) 0.086(5) 0.012(4) 0.023(4) 0.009(4)
C11 0.077(5) 0.071(4) 0.051(4) 0.003(3) 0.009(3) 0.022(3)
C12 0.072(5) 0.189(10) 0.059(4) 0.033(5) 0.022(4) 0.071(6)
C13 0.094(6) 0.104(6) 0.097(6) 0.038(5) 0.020(5) 0.017(5)
C14 0.067(4) 0.084(5) 0.084(5) 0.000(4) 0.019(4) -0.004(4)
C1A 0.049(3) 0.082(4) 0.023(2) -0.006(3) 0.006(2) -0.008(3)
N1' 0.027(2) 0.067(3) 0.0216(18) -0.0009(18) 0.0045(15) 0.0075(19)
N2' 0.033(2) 0.072(3) 0.025(2) 0.0011(19) 0.0076(16) 0.007(2)
N3' 0.036(2) 0.066(3) 0.026(2) 0.0026(19) 0.0072(16) 0.010(2)
C4' 0.037(3) 0.080(4) 0.024(2) 0.004(2) 0.007(2) 0.005(3)
C5' 0.031(2) 0.076(4) 0.020(2) 0.001(2) 0.0063(18) 0.001(2)
C6' 0.034(3) 0.066(4) 0.049(3) 0.010(3) 0.012(2) 0.012(2)
C7' 0.065(4) 0.075(5) 0.061(4) -0.002(3) 0.018(3) 0.002(3)
C8' 0.087(6) 0.074(5) 0.091(6) -0.001(4) 0.011(5) -0.003(4)
C9' 0.061(4) 0.069(5) 0.100(6) 0.016(4) 0.031(4) 0.006(3)
C10' 0.058(4) 0.082(5) 0.080(5) 0.030(4) 0.029(4) 0.014(4)
C11' 0.056(4) 0.079(4) 0.054(3) 0.012(3) 0.023(3) 0.011(3)
C1B 0.033(3) 0.076(4) 0.026(2) 0.003(2) 0.011(2) 0.011(2)
C2B 0.045(3) 0.081(4) 0.024(2) 0.011(2) 0.015(2) 0.021(3)
C3B 0.039(3) 0.101(5) 0.017(2) -0.004(3) 0.006(2) 0.024(3)
C4B 0.038(3) 0.075(4) 0.030(2) -0.004(2) 0.011(2) 0.012(3)
C5B 0.030(2) 0.072(4) 0.022(2) -0.003(2) 0.0052(18) 0.015(2)
C6B 0.049(3) 0.099(5) 0.049(3) -0.003(3) 0.017(3) -0.007(3)
C7B 0.069(4) 0.099(5) 0.046(3) 0.029(3) 0.033(3) 0.030(4)
C8B 0.064(4) 0.166(8) 0.022(3) -0.017(4) -0.003(3) 0.022(5)
C9B 0.059(4) 0.082(5) 0.058(4) -0.018(3) 0.018(3) 0.007(3)
C10B 0.047(3) 0.093(5) 0.034(3) 0.011(3) 0.006(2) 0.023(3)
B1C 0.044(3) 0.039(3) 0.025(2) -0.001(2) 0.009(2) 0.002(2)
C11C 0.034(2) 0.041(3) 0.024(2) -0.0020(19) 0.0108(18) 0.002(2)
C12C 0.038(3) 0.046(3) 0.028(2) -0.002(2) 0.0090(19) -0.002(2)
C13C 0.043(3) 0.056(3) 0.031(2) 0.008(2) 0.007(2) 0.004(2)
C14C 0.038(3) 0.069(4) 0.027(2) -0.004(2) 0.004(2) 0.002(3)
C15C 0.040(3) 0.055(3) 0.038(3) -0.012(2) 0.011(2) -0.004(2)
C16C 0.043(3) 0.043(3) 0.030(2) -0.002(2) 0.013(2) 0.002(2)
C21C 0.037(2) 0.042(3) 0.024(2) -0.0020(19) 0.0039(18) 0.002(2)
C22C 0.063(3) 0.055(3) 0.028(2) 0.002(2) 0.012(2) 0.012(3)
C23C 0.057(3) 0.055(3) 0.040(3) -0.007(2) 0.009(2) 0.015(3)
C24C 0.053(3) 0.039(3) 0.044(3) -0.001(2) -0.009(2) 0.003(2)
C25C 0.042(3) 0.050(3) 0.030(2) 0.005(2) -0.004(2) -0.002(2)
C26C 0.035(2) 0.041(3) 0.025(2) -0.0017(19) -0.0004(18) -0.003(2)
C31C 0.048(3) 0.048(3) 0.017(2) 0.0008(19) 0.0056(19) -0.002(2)
C32C 0.051(3) 0.070(4) 0.022(2) 0.005(2) 0.008(2) -0.010(3)
C33C 0.057(4) 0.096(5) 0.030(3) 0.003(3) 0.013(2) -0.023(3)
C34C 0.081(5) 0.091(5) 0.029(3) -0.002(3) 0.012(3) -0.049(4)
C35C 0.095(5) 0.056(3) 0.028(3) -0.002(2) 0.007(3) -0.026(3)
C36C 0.064(3) 0.050(3) 0.026(2) -0.001(2) 0.002(2) -0.012(3)
C41C 0.055(3) 0.035(2) 0.027(2) 0.0056(19) 0.014(2) 0.008(2)
C42C 0.059(3) 0.044(3) 0.026(2) -0.001(2) 0.008(2) 0.011(2)
C43C 0.078(4) 0.042(3) 0.030(3) -0.001(2) 0.016(3) 0.016(3)
C44C 0.081(5) 0.057(3) 0.039(3) 0.009(2) 0.032(3) 0.020(3)
C45C 0.060(4) 0.076(4) 0.054(4) -0.004(3) 0.031(3) -0.003(3)
C46C 0.055(3) 0.061(4) 0.039(3) -0.008(3) 0.022(2) -0.002(3)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1D Cl2D 1.750(10) . ?
C1D Cl1D 1.753(11) . ?
C1D H1D1 0.9900 . ?
C1D H1D2 0.9900 . ?
Rh1 C2 2.067(6) . ?
Rh1 N1' 2.138(4) . ?
Rh1 C5B 2.147(5) . ?
Rh1 C2B 2.167(5) . ?
Rh1 C1B 2.188(5) . ?
Rh1 C4B 2.188(6) . ?
Rh1 C3B 2.211(5) . ?
Rh1 Cl1 2.4094(11) . ?
N1 C2 1.340(8) . ?
N1 C5 1.421(8) . ?
N1 C6 1.435(8) . ?
C2 N3 1.371(7) . ?
N3 C4 1.363(8) . ?
N3 C1A 1.449(8) . ?
C4 C5 1.312(10) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 C7 1.311(10) . ?
C6 C11 1.485(10) . ?
C7 C8 1.405(10) . ?
C7 C12 1.573(11) . ?
C8 C9 1.396(11) . ?
C8 H8 0.9500 . ?
C9 C10 1.379(11) . ?
C9 C13 1.509(11) . ?
C10 C11 1.349(10) . ?
C10 H10 0.9500 . ?
C11 C14 1.461(10) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C1A C5' 1.471(8) . ?
C1A H1A1 0.9900 . ?
C1A H1A2 0.9900 . ?
N1' N2' 1.309(6) . ?
N1' C5' 1.346(6) . ?
N2' N3' 1.349(6) . ?
N3' C4' 1.342(7) . ?
N3' C6' 1.431(7) . ?
C4' C5' 1.357(8) . ?
C4' H4' 0.9500 . ?
C6' C7' 1.357(9) . ?
C6' C11' 1.392(8) . ?
C7' C8' 1.403(11) . ?
C7' H7' 0.9500 . ?
C8' C9' 1.376(12) . ?
C8' H8' 0.9500 . ?
C9' C10' 1.369(11) . ?
C9' H9' 0.9500 . ?
C10' C11' 1.400(10) . ?
C10' H10' 0.9500 . ?
C11' H11' 0.9500 . ?
C1B C5B 1.399(8) . ?
C1B C2B 1.451(7) . ?
C1B C6B 1.477(8) . ?
C2B C3B 1.427(9) . ?
C2B C7B 1.497(8) . ?
C3B C4B 1.408(8) . ?
C3B C8B 1.495(7) . ?
C4B C5B 1.448(7) . ?
C4B C9B 1.488(9) . ?
C5B C10B 1.498(7) . ?
C6B H6B1 0.9800 . ?
C6B H6B2 0.9800 . ?
C6B H6B3 0.9800 . ?
C7B H7B1 0.9800 . ?
C7B H7B2 0.9800 . ?
C7B H7B3 0.9800 . ?
C8B H8B1 0.9800 . ?
C8B H8B2 0.9800 . ?
C8B H8B3 0.9800 . ?
C9B H9B1 0.9800 . ?
C9B H9B2 0.9800 . ?
C9B H9B3 0.9800 . ?
C10B H10A 0.9800 . ?
C10B H10B 0.9800 . ?
C10B H10C 0.9800 . ?
B1C C41C 1.649(7) . ?
B1C C31C 1.647(8) . ?
B1C C11C 1.659(7) . ?
B1C C21C 1.652(7) . ?
C11C C12C 1.402(7) . ?
C11C C16C 1.409(7) . ?
C12C C13C 1.395(7) . ?
C12C H12D 0.9500 . ?
C13C C14C 1.394(8) . ?
C13C H13D 0.9500 . ?
C14C C15C 1.376(8) . ?
C14C H14D 0.9500 . ?
C15C C16C 1.386(7) . ?
C15C H15C 0.9500 . ?
C16C H16C 0.9500 . ?
C21C C26C 1.399(6) . ?
C21C C22C 1.411(7) . ?
C22C C23C 1.383(8) . ?
C22C H22C 0.9500 . ?
C23C C24C 1.388(8) . ?
C23C H23C 0.9500 . ?
C24C C25C 1.374(8) . ?
C24C H24C 0.9500 . ?
C25C C26C 1.388(7) . ?
C25C H25C 0.9500 . ?
C26C H26C 0.9500 . ?
C31C C32C 1.384(8) . ?
C31C C36C 1.411(8) . ?
C32C C33C 1.402(8) . ?
C32C H32C 0.9500 . ?
C33C C34C 1.382(10) . ?
C33C H33C 0.9500 . ?
C34C C35C 1.380(10) . ?
C34C H34C 0.9500 . ?
C35C C36C 1.394(8) . ?
C35C H35C 0.9500 . ?
C36C H36C 0.9500 . ?
C41C C42C 1.392(7) . ?
C41C C46C 1.397(8) . ?
C42C C43C 1.412(7) . ?
C42C H42C 0.9500 . ?
C43C C44C 1.364(9) . ?
C43C H43C 0.9500 . ?
C44C C45C 1.375(9) . ?
C44C H44C 0.9500 . ?
C45C C46C 1.396(8) . ?
C45C H45C 0.9500 . ?
C46C H46C 0.9500 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl2D C1D Cl1D 111.3(9) . . ?
Cl2D C1D H1D1 109.4 . . ?
Cl1D C1D H1D1 109.4 . . ?
Cl2D C1D H1D2 109.4 . . ?
Cl1D C1D H1D2 109.4 . . ?
H1D1 C1D H1D2 108.0 . . ?
C2 Rh1 N1' 83.97(19) . . ?
C2 Rh1 C5B 122.7(2) . . ?
N1' Rh1 C5B 91.82(17) . . ?
C2 Rh1 C2B 110.1(2) . . ?
N1' Rh1 C2B 155.90(18) . . ?
C5B Rh1 C2B 64.18(19) . . ?
C2 Rh1 C1B 99.9(2) . . ?
N1' Rh1 C1B 121.34(17) . . ?
C5B Rh1 C1B 37.6(2) . . ?
C2B Rh1 C1B 38.93(19) . . ?
C2 Rh1 C4B 161.6(2) . . ?
N1' Rh1 C4B 96.12(18) . . ?
C5B Rh1 C4B 39.01(19) . . ?
C2B Rh1 C4B 64.3(2) . . ?
C1B Rh1 C4B 64.4(2) . . ?
C2 Rh1 C3B 145.7(2) . . ?
N1' Rh1 C3B 130.3(2) . . ?
C5B Rh1 C3B 63.18(18) . . ?
C2B Rh1 C3B 38.0(2) . . ?
C1B Rh1 C3B 63.5(2) . . ?
C4B Rh1 C3B 37.3(2) . . ?
C2 Rh1 Cl1 91.84(17) . . ?
N1' Rh1 Cl1 89.93(11) . . ?
C5B Rh1 Cl1 145.44(15) . . ?
C2B Rh1 Cl1 108.45(15) . . ?
C1B Rh1 Cl1 147.38(13) . . ?
C4B Rh1 Cl1 106.51(15) . . ?
C3B Rh1 Cl1 89.95(14) . . ?
C2 N1 C5 109.3(5) . . ?
C2 N1 C6 129.6(5) . . ?
C5 N1 C6 119.8(6) . . ?
N1 C2 N3 103.3(5) . . ?
N1 C2 Rh1 135.9(4) . . ?
N3 C2 Rh1 120.6(4) . . ?
C4 N3 C2 113.5(5) . . ?
C4 N3 C1A 121.7(5) . . ?
C2 N3 C1A 124.7(5) . . ?
C5 C4 N3 105.1(6) . . ?
C5 C4 H4 127.5 . . ?
N3 C4 H4 127.5 . . ?
C4 C5 N1 108.8(6) . . ?
C4 C5 H5 125.6 . . ?
N1 C5 H5 125.6 . . ?
C7 C6 N1 119.9(6) . . ?
C7 C6 C11 125.0(6) . . ?
N1 C6 C11 113.5(6) . . ?
C6 C7 C8 116.5(7) . . ?
C6 C7 C12 123.6(6) . . ?
C8 C7 C12 119.8(6) . . ?
C7 C8 C9 122.1(7) . . ?
C7 C8 H8 119.0 . . ?
C9 C8 H8 119.0 . . ?
C10 C9 C8 118.1(7) . . ?
C10 C9 C13 121.3(7) . . ?
C8 C9 C13 120.5(7) . . ?
C9 C10 C11 124.0(7) . . ?
C9 C10 H10 118.0 . . ?
C11 C10 H10 118.0 . . ?
C10 C11 C14 124.4(7) . . ?
C10 C11 C6 113.9(6) . . ?
C14 C11 C6 121.7(6) . . ?
C7 C12 H12A 109.5 . . ?
C7 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C7 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C9 C13 H13A 109.5 . . ?
C9 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C9 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N3 C1A C5' 110.5(5) . . ?
N3 C1A H1A1 109.6 . . ?
C5' C1A H1A1 109.6 . . ?
N3 C1A H1A2 109.6 . . ?
C5' C1A H1A2 109.6 . . ?
H1A1 C1A H1A2 108.1 . . ?
N2' N1' C5' 111.0(4) . . ?
N2' N1' Rh1 125.6(3) . . ?
C5' N1' Rh1 122.5(4) . . ?
N1' N2' N3' 105.2(4) . . ?
N2' N3' C4' 111.2(4) . . ?
N2' N3' C6' 119.5(4) . . ?
C4' N3' C6' 129.3(4) . . ?
N3' C4' C5' 105.3(4) . . ?
N3' C4' H4' 127.3 . . ?
C5' C4' H4' 127.3 . . ?
N1' C5' C4' 107.3(5) . . ?
N1' C5' C1A 121.0(4) . . ?
C4' C5' C1A 131.6(5) . . ?
C7' C6' C11' 121.2(6) . . ?
C7' C6' N3' 120.1(5) . . ?
C11' C6' N3' 118.7(6) . . ?
C6' C7' C8' 119.0(7) . . ?
C6' C7' H7' 120.5 . . ?
C8' C7' H7' 120.5 . . ?
C9' C8' C7' 120.8(8) . . ?
C9' C8' H8' 119.6 . . ?
C7' C8' H8' 119.6 . . ?
C10' C9' C8' 119.7(7) . . ?
C10' C9' H9' 120.2 . . ?
C8' C9' H9' 120.2 . . ?
C9' C10' C11' 120.3(7) . . ?
C9' C10' H10' 119.8 . . ?
C11' C10' H10' 119.8 . . ?
C6' C11' C10' 118.9(7) . . ?
C6' C11' H11' 120.5 . . ?
C10' C11' H11' 120.5 . . ?
C5B C1B C2B 107.0(5) . . ?
C5B C1B C6B 123.5(5) . . ?
C2B C1B C6B 129.0(6) . . ?
C5B C1B Rh1 69.6(3) . . ?
C2B C1B Rh1 69.8(3) . . ?
C6B C1B Rh1 131.6(4) . . ?
C3B C2B C1B 107.1(5) . . ?
C3B C2B C7B 124.0(5) . . ?
C1B C2B C7B 127.7(6) . . ?
C3B C2B Rh1 72.6(3) . . ?
C1B C2B Rh1 71.3(3) . . ?
C7B C2B Rh1 130.7(4) . . ?
C4B C3B C2B 109.6(5) . . ?
C4B C3B C8B 126.5(7) . . ?
C2B C3B C8B 123.9(6) . . ?
C4B C3B Rh1 70.4(3) . . ?
C2B C3B Rh1 69.3(3) . . ?
C8B C3B Rh1 127.0(4) . . ?
C3B C4B C5B 106.2(5) . . ?
C3B C4B C9B 126.4(5) . . ?
C5B C4B C9B 127.2(5) . . ?
C3B C4B Rh1 72.2(3) . . ?
C5B C4B Rh1 69.0(3) . . ?
C9B C4B Rh1 127.0(4) . . ?
C1B C5B C4B 109.9(4) . . ?
C1B C5B C10B 125.4(5) . . ?
C4B C5B C10B 124.6(5) . . ?
C1B C5B Rh1 72.8(3) . . ?
C4B C5B Rh1 72.0(3) . . ?
C10B C5B Rh1 125.1(3) . . ?
C1B C6B H6B1 109.5 . . ?
C1B C6B H6B2 109.5 . . ?
H6B1 C6B H6B2 109.5 . . ?
C1B C6B H6B3 109.5 . . ?
H6B1 C6B H6B3 109.5 . . ?
H6B2 C6B H6B3 109.5 . . ?
C2B C7B H7B1 109.5 . . ?
C2B C7B H7B2 109.5 . . ?
H7B1 C7B H7B2 109.5 . . ?
C2B C7B H7B3 109.5 . . ?
H7B1 C7B H7B3 109.5 . . ?
H7B2 C7B H7B3 109.5 . . ?
C3B C8B H8B1 109.5 . . ?
C3B C8B H8B2 109.5 . . ?
H8B1 C8B H8B2 109.5 . . ?
C3B C8B H8B3 109.5 . . ?
H8B1 C8B H8B3 109.5 . . ?
H8B2 C8B H8B3 109.5 . . ?
C4B C9B H9B1 109.5 . . ?
C4B C9B H9B2 109.5 . . ?
H9B1 C9B H9B2 109.5 . . ?
C4B C9B H9B3 109.5 . . ?
H9B1 C9B H9B3 109.5 . . ?
H9B2 C9B H9B3 109.5 . . ?
C5B C10B H10A 109.5 . . ?
C5B C10B H10B 109.5 . . ?
H10A C10B H10B 109.5 . . ?
C5B C10B H10C 109.5 . . ?
H10A C10B H10C 109.5 . . ?
H10B C10B H10C 109.5 . . ?
C41C B1C C31C 110.6(4) . . ?
C41C B1C C11C 109.0(4) . . ?
C31C B1C C11C 109.2(4) . . ?
C41C B1C C21C 108.2(4) . . ?
C31C B1C C21C 111.5(4) . . ?
C11C B1C C21C 108.2(4) . . ?
C12C C11C C16C 114.8(4) . . ?
C12C C11C B1C 123.5(4) . . ?
C16C C11C B1C 121.7(4) . . ?
C13C C12C C11C 123.1(5) . . ?
C13C C12C H12D 118.4 . . ?
C11C C12C H12D 118.4 . . ?
C12C C13C C14C 119.8(5) . . ?
C12C C13C H13D 120.1 . . ?
C14C C13C H13D 120.1 . . ?
C15C C14C C13C 118.7(5) . . ?
C15C C14C H14D 120.7 . . ?
C13C C14C H14D 120.7 . . ?
C14C C15C C16C 120.9(5) . . ?
C14C C15C H15C 119.6 . . ?
C16C C15C H15C 119.6 . . ?
C15C C16C C11C 122.7(5) . . ?
C15C C16C H16C 118.6 . . ?
C11C C16C H16C 118.6 . . ?
C26C C21C C22C 113.8(4) . . ?
C26C C21C B1C 124.2(4) . . ?
C22C C21C B1C 121.9(4) . . ?
C23C C22C C21C 123.8(5) . . ?
C23C C22C H22C 118.1 . . ?
C21C C22C H22C 118.1 . . ?
C22C C23C C24C 119.7(5) . . ?
C22C C23C H23C 120.1 . . ?
C24C C23C H23C 120.1 . . ?
C25C C24C C23C 118.7(5) . . ?
C25C C24C H24C 120.6 . . ?
C23C C24C H24C 120.6 . . ?
C24C C25C C26C 120.7(5) . . ?
C24C C25C H25C 119.7 . . ?
C26C C25C H25C 119.7 . . ?
C25C C26C C21C 123.2(4) . . ?
C25C C26C H26C 118.4 . . ?
C21C C26C H26C 118.4 . . ?
C32C C31C C36C 115.3(5) . . ?
C32C C31C B1C 124.5(5) . . ?
C36C C31C B1C 120.2(5) . . ?
C31C C32C C33C 123.3(6) . . ?
C31C C32C H32C 118.4 . . ?
C33C C32C H32C 118.4 . . ?
C34C C33C C32C 119.9(6) . . ?
C34C C33C H33C 120.0 . . ?
C32C C33C H33C 120.0 . . ?
C35C C34C C33C 118.5(6) . . ?
C35C C34C H34C 120.8 . . ?
C33C C34C H34C 120.8 . . ?
C34C C35C C36C 121.1(6) . . ?
C34C C35C H35C 119.4 . . ?
C36C C35C H35C 119.4 . . ?
C35C C36C C31C 121.9(6) . . ?
C35C C36C H36C 119.1 . . ?
C31C C36C H36C 119.1 . . ?
C42C C41C C46C 114.9(5) . . ?
C42C C41C B1C 123.5(5) . . ?
C46C C41C B1C 121.4(4) . . ?
C41C C42C C43C 122.3(6) . . ?
C41C C42C H42C 118.8 . . ?
C43C C42C H42C 118.8 . . ?
C44C C43C C42C 120.2(5) . . ?
C44C C43C H43C 119.9 . . ?
C42C C43C H43C 119.9 . . ?
C45C C44C C43C 119.6(5) . . ?
C45C C44C H44C 120.2 . . ?
C43C C44C H44C 120.2 . . ?
C44C C45C C46C 119.6(6) . . ?
C44C C45C H45C 120.2 . . ?
C46C C45C H45C 120.2 . . ?
C45C C46C C41C 123.3(6) . . ?
C45C C46C H46C 118.3 . . ?
C41C C46C H46C 118.3 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 C2 N3 -0.3(6) . . . . ?
C6 N1 C2 N3 166.2(6) . . . . ?
C5 N1 C2 Rh1 173.4(5) . . . . ?
C6 N1 C2 Rh1 -20.1(10) . . . . ?
N1' Rh1 C2 N1 -139.1(6) . . . . ?
C5B Rh1 C2 N1 132.6(5) . . . . ?
C2B Rh1 C2 N1 61.1(6) . . . . ?
C1B Rh1 C2 N1 100.1(6) . . . . ?
C4B Rh1 C2 N1 129.6(7) . . . . ?
C3B Rh1 C2 N1 43.3(8) . . . . ?
Cl1 Rh1 C2 N1 -49.4(6) . . . . ?
N1' Rh1 C2 N3 33.8(4) . . . . ?
C5B Rh1 C2 N3 -54.5(5) . . . . ?
C2B Rh1 C2 N3 -126.1(4) . . . . ?
C1B Rh1 C2 N3 -87.0(4) . . . . ?
C4B Rh1 C2 N3 -57.5(8) . . . . ?
C3B Rh1 C2 N3 -143.9(4) . . . . ?
Cl1 Rh1 C2 N3 123.5(4) . . . . ?
N1 C2 N3 C4 -0.6(6) . . . . ?
Rh1 C2 N3 C4 -175.5(4) . . . . ?
N1 C2 N3 C1A -178.7(5) . . . . ?
Rh1 C2 N3 C1A 6.4(7) . . . . ?
C2 N3 C4 C5 1.2(7) . . . . ?
C1A N3 C4 C5 179.4(5) . . . . ?
N3 C4 C5 N1 -1.3(7) . . . . ?
C2 N1 C5 C4 1.0(7) . . . . ?
C6 N1 C5 C4 -167.0(6) . . . . ?
C2 N1 C6 C7 111.6(8) . . . . ?
C5 N1 C6 C7 -83.2(10) . . . . ?
C2 N1 C6 C11 -82.4(9) . . . . ?
C5 N1 C6 C11 82.9(7) . . . . ?
N1 C6 C7 C8 171.1(8) . . . . ?
C11 C6 C7 C8 6.8(13) . . . . ?
N1 C6 C7 C12 -9.5(14) . . . . ?
C11 C6 C7 C12 -173.9(8) . . . . ?
C6 C7 C8 C9 -0.9(14) . . . . ?
C12 C7 C8 C9 179.8(9) . . . . ?
C7 C8 C9 C10 -4.0(15) . . . . ?
C7 C8 C9 C13 -178.7(9) . . . . ?
C8 C9 C10 C11 3.1(14) . . . . ?
C13 C9 C10 C11 177.8(9) . . . . ?
C9 C10 C11 C14 -177.9(8) . . . . ?
C9 C10 C11 C6 2.1(12) . . . . ?
C7 C6 C11 C10 -7.5(12) . . . . ?
N1 C6 C11 C10 -172.7(6) . . . . ?
C7 C6 C11 C14 172.5(8) . . . . ?
N1 C6 C11 C14 7.3(10) . . . . ?
C4 N3 C1A C5' 125.5(5) . . . . ?
C2 N3 C1A C5' -56.5(7) . . . . ?
C2 Rh1 N1' N2' 150.7(4) . . . . ?
C5B Rh1 N1' N2' -86.6(4) . . . . ?
C2B Rh1 N1' N2' -81.7(6) . . . . ?
C1B Rh1 N1' N2' -111.3(4) . . . . ?
C4B Rh1 N1' N2' -47.7(4) . . . . ?
C3B Rh1 N1' N2' -31.0(4) . . . . ?
Cl1 Rh1 N1' N2' 58.9(4) . . . . ?
C2 Rh1 N1' C5' -41.0(4) . . . . ?
C5B Rh1 N1' C5' 81.7(4) . . . . ?
C2B Rh1 N1' C5' 86.6(6) . . . . ?
C1B Rh1 N1' C5' 56.9(5) . . . . ?
C4B Rh1 N1' C5' 120.6(4) . . . . ?
C3B Rh1 N1' C5' 137.3(4) . . . . ?
Cl1 Rh1 N1' C5' -132.8(4) . . . . ?
C5' N1' N2' N3' 0.3(5) . . . . ?
Rh1 N1' N2' N3' 169.8(3) . . . . ?
N1' N2' N3' C4' -0.1(5) . . . . ?
N1' N2' N3' C6' -178.6(4) . . . . ?
N2' N3' C4' C5' -0.2(6) . . . . ?
C6' N3' C4' C5' 178.2(5) . . . . ?
N2' N1' C5' C4' -0.4(6) . . . . ?
Rh1 N1' C5' C4' -170.3(3) . . . . ?
N2' N1' C5' C1A 176.4(5) . . . . ?
Rh1 N1' C5' C1A 6.6(7) . . . . ?
N3' C4' C5' N1' 0.4(6) . . . . ?
N3' C4' C5' C1A -176.0(6) . . . . ?
N3 C1A C5' N1' 47.3(7) . . . . ?
N3 C1A C5' C4' -136.7(6) . . . . ?
N2' N3' C6' C7' 18.0(7) . . . . ?
C4' N3' C6' C7' -160.2(6) . . . . ?
N2' N3' C6' C11' -162.5(5) . . . . ?
C4' N3' C6' C11' 19.3(8) . . . . ?
C11' C6' C7' C8' 0.7(10) . . . . ?
N3' C6' C7' C8' -179.8(6) . . . . ?
C6' C7' C8' C9' -0.7(12) . . . . ?
C7' C8' C9' C10' -1.0(12) . . . . ?
C8' C9' C10' C11' 2.8(11) . . . . ?
C7' C6' C11' C10' 1.1(9) . . . . ?
N3' C6' C11' C10' -178.5(5) . . . . ?
C9' C10' C11' C6' -2.8(10) . . . . ?
C2 Rh1 C1B C5B 132.2(3) . . . . ?
N1' Rh1 C1B C5B 43.2(3) . . . . ?
C2B Rh1 C1B C5B -118.0(5) . . . . ?
C4B Rh1 C1B C5B -37.9(3) . . . . ?
C3B Rh1 C1B C5B -79.6(3) . . . . ?
Cl1 Rh1 C1B C5B -118.4(3) . . . . ?
C2 Rh1 C1B C2B -109.8(4) . . . . ?
N1' Rh1 C1B C2B 161.3(3) . . . . ?
C5B Rh1 C1B C2B 118.0(5) . . . . ?
C4B Rh1 C1B C2B 80.1(4) . . . . ?
C3B Rh1 C1B C2B 38.4(4) . . . . ?
Cl1 Rh1 C1B C2B -0.4(5) . . . . ?
C2 Rh1 C1B C6B 14.9(6) . . . . ?
N1' Rh1 C1B C6B -74.0(6) . . . . ?
C5B Rh1 C1B C6B -117.2(7) . . . . ?
C2B Rh1 C1B C6B 124.8(7) . . . . ?
C4B Rh1 C1B C6B -155.1(6) . . . . ?
C3B Rh1 C1B C6B 163.1(6) . . . . ?
Cl1 Rh1 C1B C6B 124.4(5) . . . . ?
C5B C1B C2B C3B -4.4(5) . . . . ?
C6B C1B C2B C3B 168.0(5) . . . . ?
Rh1 C1B C2B C3B -64.3(3) . . . . ?
C5B C1B C2B C7B -172.6(5) . . . . ?
C6B C1B C2B C7B -0.2(9) . . . . ?
Rh1 C1B C2B C7B 127.5(6) . . . . ?
C5B C1B C2B Rh1 59.9(3) . . . . ?
C6B C1B C2B Rh1 -127.7(6) . . . . ?
C2 Rh1 C2B C3B -163.7(3) . . . . ?
N1' Rh1 C2B C3B 73.3(6) . . . . ?
C5B Rh1 C2B C3B 78.8(3) . . . . ?
C1B Rh1 C2B C3B 115.6(5) . . . . ?
C4B Rh1 C2B C3B 35.2(3) . . . . ?
Cl1 Rh1 C2B C3B -64.6(3) . . . . ?
C2 Rh1 C2B C1B 80.7(4) . . . . ?
N1' Rh1 C2B C1B -42.2(7) . . . . ?
C5B Rh1 C2B C1B -36.8(3) . . . . ?
C4B Rh1 C2B C1B -80.3(4) . . . . ?
C3B Rh1 C2B C1B -115.6(5) . . . . ?
Cl1 Rh1 C2B C1B 179.8(3) . . . . ?
C2 Rh1 C2B C7B -43.4(7) . . . . ?
N1' Rh1 C2B C7B -166.4(5) . . . . ?
C5B Rh1 C2B C7B -160.9(7) . . . . ?
C1B Rh1 C2B C7B -124.1(8) . . . . ?
C4B Rh1 C2B C7B 155.6(7) . . . . ?
C3B Rh1 C2B C7B 120.3(7) . . . . ?
Cl1 Rh1 C2B C7B 55.7(7) . . . . ?
C1B C2B C3B C4B 4.3(6) . . . . ?
C7B C2B C3B C4B 173.1(5) . . . . ?
Rh1 C2B C3B C4B -59.0(3) . . . . ?
C1B C2B C3B C8B -175.2(5) . . . . ?
C7B C2B C3B C8B -6.4(8) . . . . ?
Rh1 C2B C3B C8B 121.4(5) . . . . ?
C1B C2B C3B Rh1 63.4(3) . . . . ?
C7B C2B C3B Rh1 -127.8(5) . . . . ?
C2 Rh1 C3B C4B 148.8(4) . . . . ?
N1' Rh1 C3B C4B -28.2(4) . . . . ?
C5B Rh1 C3B C4B 39.4(3) . . . . ?
C2B Rh1 C3B C4B 121.0(4) . . . . ?
C1B Rh1 C3B C4B 81.7(3) . . . . ?
Cl1 Rh1 C3B C4B -118.0(3) . . . . ?
C2 Rh1 C3B C2B 27.8(5) . . . . ?
N1' Rh1 C3B C2B -149.1(3) . . . . ?
C5B Rh1 C3B C2B -81.6(3) . . . . ?
C1B Rh1 C3B C2B -39.3(3) . . . . ?
C4B Rh1 C3B C2B -121.0(4) . . . . ?
Cl1 Rh1 C3B C2B 121.0(3) . . . . ?
C2 Rh1 C3B C8B -89.7(8) . . . . ?
N1' Rh1 C3B C8B 93.3(7) . . . . ?
C5B Rh1 C3B C8B 160.9(8) . . . . ?
C2B Rh1 C3B C8B -117.5(8) . . . . ?
C1B Rh1 C3B C8B -156.8(8) . . . . ?
C4B Rh1 C3B C8B 121.5(8) . . . . ?
Cl1 Rh1 C3B C8B 3.5(7) . . . . ?
C2B C3B C4B C5B -2.6(5) . . . . ?
C8B C3B C4B C5B 176.9(5) . . . . ?
Rh1 C3B C4B C5B -61.0(3) . . . . ?
C2B C3B C4B C9B -178.4(5) . . . . ?
C8B C3B C4B C9B 1.1(9) . . . . ?
Rh1 C3B C4B C9B 123.3(5) . . . . ?
C2B C3B C4B Rh1 58.4(4) . . . . ?
C8B C3B C4B Rh1 -122.1(5) . . . . ?
C2 Rh1 C4B C3B -111.9(6) . . . . ?
N1' Rh1 C4B C3B 158.8(3) . . . . ?
C5B Rh1 C4B C3B -115.9(5) . . . . ?
C2B Rh1 C4B C3B -35.9(3) . . . . ?
C1B Rh1 C4B C3B -79.3(4) . . . . ?
Cl1 Rh1 C4B C3B 67.0(3) . . . . ?
C2 Rh1 C4B C5B 4.0(8) . . . . ?
N1' Rh1 C4B C5B -85.3(3) . . . . ?
C2B Rh1 C4B C5B 80.0(3) . . . . ?
C1B Rh1 C4B C5B 36.6(3) . . . . ?
C3B Rh1 C4B C5B 115.9(5) . . . . ?
Cl1 Rh1 C4B C5B -177.1(3) . . . . ?
C2 Rh1 C4B C9B 125.4(7) . . . . ?
N1' Rh1 C4B C9B 36.1(5) . . . . ?
C5B Rh1 C4B C9B 121.5(6) . . . . ?
C2B Rh1 C4B C9B -158.5(6) . . . . ?
C1B Rh1 C4B C9B 158.1(6) . . . . ?
C3B Rh1 C4B C9B -122.6(6) . . . . ?
Cl1 Rh1 C4B C9B -55.6(5) . . . . ?
C2B C1B C5B C4B 2.9(5) . . . . ?
C6B C1B C5B C4B -170.0(5) . . . . ?
Rh1 C1B C5B C4B 62.9(3) . . . . ?
C2B C1B C5B C10B 178.8(5) . . . . ?
C6B C1B C5B C10B 5.9(8) . . . . ?
Rh1 C1B C5B C10B -121.2(5) . . . . ?
C2B C1B C5B Rh1 -60.0(3) . . . . ?
C6B C1B C5B Rh1 127.1(5) . . . . ?
C3B C4B C5B C1B -0.2(5) . . . . ?
C9B C4B C5B C1B 175.5(5) . . . . ?
Rh1 C4B C5B C1B -63.4(3) . . . . ?
C3B C4B C5B C10B -176.2(4) . . . . ?
C9B C4B C5B C10B -0.5(8) . . . . ?
Rh1 C4B C5B C10B 120.7(5) . . . . ?
C3B C4B C5B Rh1 63.1(3) . . . . ?
C9B C4B C5B Rh1 -121.1(5) . . . . ?
C2 Rh1 C5B C1B -60.2(3) . . . . ?
N1' Rh1 C5B C1B -144.2(3) . . . . ?
C2B Rh1 C5B C1B 38.0(3) . . . . ?
C4B Rh1 C5B C1B 118.3(4) . . . . ?
C3B Rh1 C5B C1B 80.7(3) . . . . ?
Cl1 Rh1 C5B C1B 123.3(3) . . . . ?
C2 Rh1 C5B C4B -178.5(3) . . . . ?
N1' Rh1 C5B C4B 97.5(3) . . . . ?
C2B Rh1 C5B C4B -80.3(3) . . . . ?
C1B Rh1 C5B C4B -118.3(4) . . . . ?
C3B Rh1 C5B C4B -37.7(3) . . . . ?
Cl1 Rh1 C5B C4B 5.0(4) . . . . ?
C2 Rh1 C5B C10B 61.4(6) . . . . ?
N1' Rh1 C5B C10B -22.6(5) . . . . ?
C2B Rh1 C5B C10B 159.6(6) . . . . ?
C1B Rh1 C5B C10B 121.6(6) . . . . ?
C4B Rh1 C5B C10B -120.1(7) . . . . ?
C3B Rh1 C5B C10B -157.8(6) . . . . ?
Cl1 Rh1 C5B C10B -115.1(5) . . . . ?
C41C B1C C11C C12C 93.1(5) . . . . ?
C31C B1C C11C C12C -27.9(6) . . . . ?
C21C B1C C11C C12C -149.4(4) . . . . ?
C41C B1C C11C C16C -84.3(5) . . . . ?
C31C B1C C11C C16C 154.7(4) . . . . ?
C21C B1C C11C C16C 33.1(6) . . . . ?
C16C C11C C12C C13C 0.9(7) . . . . ?
B1C C11C C12C C13C -176.7(4) . . . . ?
C11C C12C C13C C14C 0.2(8) . . . . ?
C12C C13C C14C C15C -0.7(8) . . . . ?
C13C C14C C15C C16C 0.0(8) . . . . ?
C14C C15C C16C C11C 1.2(8) . . . . ?
C12C C11C C16C C15C -1.6(7) . . . . ?
B1C C11C C16C C15C 176.0(4) . . . . ?
C41C B1C C21C C26C -10.3(6) . . . . ?
C31C B1C C21C C26C 111.5(5) . . . . ?
C11C B1C C21C C26C -128.3(5) . . . . ?
C41C B1C C21C C22C 165.7(5) . . . . ?
C31C B1C C21C C22C -72.5(6) . . . . ?
C11C B1C C21C C22C 47.7(6) . . . . ?
C26C C21C C22C C23C -0.2(8) . . . . ?
B1C C21C C22C C23C -176.6(5) . . . . ?
C21C C22C C23C C24C 0.8(9) . . . . ?
C22C C23C C24C C25C -0.5(8) . . . . ?
C23C C24C C25C C26C -0.3(8) . . . . ?
C24C C25C C26C C21C 1.0(7) . . . . ?
C22C C21C C26C C25C -0.7(7) . . . . ?
B1C C21C C26C C25C 175.6(4) . . . . ?
C41C B1C C31C C32C 138.8(5) . . . . ?
C11C B1C C31C C32C -101.1(5) . . . . ?
C21C B1C C31C C32C 18.4(6) . . . . ?
C41C B1C C31C C36C -44.0(6) . . . . ?
C11C B1C C31C C36C 76.1(5) . . . . ?
C21C B1C C31C C36C -164.4(4) . . . . ?
C36C C31C C32C C33C -0.1(7) . . . . ?
B1C C31C C32C C33C 177.2(4) . . . . ?
C31C C32C C33C C34C 0.1(8) . . . . ?
C32C C33C C34C C35C -0.5(8) . . . . ?
C33C C34C C35C C36C 0.8(8) . . . . ?
C34C C35C C36C C31C -0.8(8) . . . . ?
C32C C31C C36C C35C 0.4(7) . . . . ?
B1C C31C C36C C35C -177.0(4) . . . . ?
C31C B1C C41C C42C -28.9(6) . . . . ?
C11C B1C C41C C42C -149.0(5) . . . . ?
C21C B1C C41C C42C 93.5(5) . . . . ?
C31C B1C C41C C46C 154.8(5) . . . . ?
C11C B1C C41C C46C 34.6(6) . . . . ?
C21C B1C C41C C46C -82.9(6) . . . . ?
C46C C41C C42C C43C -0.4(7) . . . . ?
B1C C41C C42C C43C -176.9(5) . . . . ?
C41C C42C C43C C44C 1.3(8) . . . . ?
C42C C43C C44C C45C -0.6(9) . . . . ?
C43C C44C C45C C46C -0.9(10) . . . . ?
C44C C45C C46C C41C 1.9(10) . . . . ?
C42C C41C C46C C45C -1.2(8) . . . . ?
B1C C41C C46C C45C 175.4(6) . . . . ?
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max 2.049
_refine_diff_density_min -0.572
_refine_diff_density_rms 0.121
_iucr_refine_instructions_details
;
TITL Marina7_P21byc in P2(1)/c
CELL 0.71073 15.2978 12.1192 26.5776 90.000 96.241 90.000
ZERR 4.00 0.0008 0.0007 0.0014 0.000 0.002 0.000
LATT 1
SYMM -X, 0.5+Y, 0.5-Z
SFAC C H B N O Rh Cl
UNIT 184 96 4 8 16 4 4
OMIT 1 0 0
OMIT 0 0 2
OMIT 1 1 0
OMIT 2 1 0
OMIT 0 1 3
OMIT -1 1 3
OMIT 1 2 0
OMIT -3 50
L.S. 25
ACTA
BOND $H
FMAP 2
PLAN 20
SIZE 0.276 0.186 0.095
CONF
SADI 0.01 C1D CL1D C1D CL2D
DELU 0.005 C1D CL1D CL2D
SIMU 0.005 C1D CL1D CL2D
TEMP -123.140
WGHT 0.117500 15.191201
FVAR 0.09363
MOLE 3
C1D 1 0.526704 0.406550 0.189195 10.50000 0.03977 0.24939 =
0.25404 -0.21013 0.03134 -0.01372
AFIX 23
H1D1 2 0.484184 0.461811 0.173860 10.50000 -1.20000
H1D2 2 0.540053 0.424586 0.225548 10.50000 -1.20000
AFIX 0
CL1D 7 0.479448 0.274802 0.183013 10.50000 0.07878 0.18792 =
0.06555 -0.00428 -0.00568 0.02311
CL2D 7 0.623399 0.413656 0.159687 10.50000 0.06751 0.14516 =
0.10232 -0.02341 0.00906 0.03322
MOLE 1
RH1 6 0.725897 0.190379 0.362478 11.00000 0.02904 0.07145 =
0.01647 0.00216 0.00595 0.01176
CL1 7 0.575986 0.209660 0.325111 11.00000 0.02135 0.15742 =
0.01684 0.00192 -0.00231 0.03291
N1 4 0.691510 0.437634 0.393897 11.00000 0.04900 0.06736 =
0.06099 0.00982 0.02908 0.00433
C2 1 0.718383 0.333861 0.403844 11.00000 0.04558 0.06509 =
0.03627 0.00406 0.02315 0.00147
N3 4 0.736305 0.332859 0.455502 11.00000 0.04569 0.06653 =
0.04125 -0.01404 0.02215 -0.00904
C4 1 0.722319 0.431893 0.477563 11.00000 0.06060 0.06700 =
0.05998 -0.00865 0.02539 -0.00617
AFIX 43
H4 2 0.731512 0.449749 0.512543 11.00000 -1.20000
AFIX 0
C5 1 0.693410 0.497239 0.440039 11.00000 0.05485 0.06621 =
0.08737 -0.02385 0.02743 0.00121
AFIX 43
H5 2 0.676516 0.572137 0.443202 11.00000 -1.20000
AFIX 0
C6 1 0.680158 0.495670 0.346585 11.00000 0.07754 0.07844 =
0.08398 0.03681 0.04747 0.03850
C7 1 0.601030 0.522532 0.326414 11.00000 0.06298 0.10914 =
0.05403 0.02470 0.00897 0.00945
C8 1 0.595877 0.592615 0.284104 11.00000 0.05305 0.11843 =
0.09941 0.02999 0.00272 0.01441
AFIX 43
H8 2 0.539620 0.613095 0.268161 11.00000 -1.20000
AFIX 0
C9 1 0.670809 0.633102 0.264752 11.00000 0.06080 0.11927 =
0.07697 0.03672 0.00730 0.00437
C10 1 0.751685 0.608027 0.290264 11.00000 0.06707 0.08299 =
0.08639 0.01183 0.02339 0.00936
AFIX 43
H10 2 0.802487 0.638644 0.278021 11.00000 -1.20000
AFIX 0
C11 1 0.763116 0.542679 0.331548 11.00000 0.07680 0.07141 =
0.05074 0.00338 0.00859 0.02180
C12 1 0.514304 0.479757 0.346701 11.00000 0.07172 0.18902 =
0.05894 0.03327 0.02162 0.07092
AFIX 137
H12A 2 0.526837 0.458795 0.382369 11.00000 -1.50000
H12B 2 0.492139 0.415462 0.326896 11.00000 -1.50000
H12C 2 0.469914 0.538369 0.343476 11.00000 -1.50000
AFIX 0
C13 1 0.662535 0.710144 0.219882 11.00000 0.09389 0.10407 =
0.09697 0.03771 0.02034 0.01668
AFIX 137
H13A 2 0.720152 0.742230 0.215823 11.00000 -1.50000
H13B 2 0.620919 0.769241 0.225430 11.00000 -1.50000
H13C 2 0.641161 0.668995 0.189254 11.00000 -1.50000
AFIX 0
C14 1 0.848328 0.518557 0.359808 11.00000 0.06699 0.08436 =
0.08401 -0.00009 0.01883 -0.00418
AFIX 137
H14A 2 0.851254 0.552693 0.393376 11.00000 -1.50000
H14B 2 0.895364 0.548293 0.341504 11.00000 -1.50000
H14C 2 0.855503 0.438511 0.363494 11.00000 -1.50000
AFIX 0
C1A 1 0.769647 0.238345 0.484999 11.00000 0.04860 0.08170 =
0.02269 -0.00563 0.00612 -0.00823
AFIX 23
H1A1 2 0.774530 0.256912 0.521472 11.00000 -1.20000
H1A2 2 0.829056 0.219298 0.476203 11.00000 -1.20000
AFIX 0
N1' 4 0.680847 0.113755 0.427358 11.00000 0.02681 0.06705 =
0.02162 -0.00090 0.00449 0.00751
N2' 4 0.633723 0.023557 0.426940 11.00000 0.03345 0.07196 =
0.02508 0.00108 0.00760 0.00671
N3' 4 0.633501 -0.004609 0.476017 11.00000 0.03583 0.06594 =
0.02625 0.00260 0.00716 0.00999
C4' 1 0.680170 0.067490 0.506458 11.00000 0.03669 0.07992 =
0.02430 0.00367 0.00732 0.00525
AFIX 43
H4' 2 0.689768 0.065919 0.542371 11.00000 -1.20000
AFIX 0
C5' 1 0.710717 0.143097 0.475005 11.00000 0.03106 0.07562 =
0.02041 0.00073 0.00626 0.00131
C6' 1 0.588636 -0.102569 0.488896 11.00000 0.03410 0.06559 =
0.04919 0.00977 0.01181 0.01182
C7' 1 0.567708 -0.181420 0.453388 11.00000 0.06508 0.07499 =
0.06093 -0.00242 0.01820 0.00189
AFIX 43
H7' 2 0.582775 -0.172369 0.419888 11.00000 -1.20000
AFIX 0
C8' 1 0.523469 -0.276545 0.466900 11.00000 0.08734 0.07363 =
0.09057 -0.00116 0.01107 -0.00290
AFIX 43
H8' 2 0.507920 -0.331816 0.442193 11.00000 -1.20000
AFIX 0
C9' 1 0.502333 -0.290753 0.515500 11.00000 0.06091 0.06938 =
0.10008 0.01599 0.03144 0.00646
AFIX 43
H9' 2 0.471545 -0.354907 0.524135 11.00000 -1.20000
AFIX 0
C10' 1 0.525886 -0.212000 0.551341 11.00000 0.05839 0.08210 =
0.08009 0.03017 0.02883 0.01403
AFIX 43
H10' 2 0.513695 -0.223146 0.585265 11.00000 -1.20000
AFIX 0
C11' 1 0.567835 -0.115136 0.538273 11.00000 0.05591 0.07909 =
0.05409 0.01219 0.02344 0.01064
AFIX 43
H11' 2 0.581884 -0.058875 0.562709 11.00000 -1.20000
AFIX 0
C1B 1 0.865488 0.192914 0.351354 11.00000 0.03298 0.07649 =
0.02650 0.00313 0.01133 0.01055
C2B 1 0.812041 0.214277 0.303830 11.00000 0.04542 0.08149 =
0.02428 0.01136 0.01506 0.02102
C3B 1 0.761626 0.117113 0.291324 11.00000 0.03869 0.10079 =
0.01711 -0.00363 0.00647 0.02386
C4B 1 0.776658 0.039718 0.330835 11.00000 0.03817 0.07454 =
0.02970 -0.00448 0.01069 0.01198
C5B 1 0.841479 0.088762 0.367924 11.00000 0.02958 0.07168 =
0.02215 -0.00254 0.00524 0.01458
C6B 1 0.939929 0.257328 0.376249 11.00000 0.04925 0.09939 =
0.04853 -0.00256 0.01725 -0.00687
AFIX 137
H6B1 2 0.993964 0.213573 0.377259 11.00000 -1.50000
H6B2 2 0.928512 0.275740 0.410840 11.00000 -1.50000
H6B3 2 0.946718 0.325425 0.357172 11.00000 -1.50000
AFIX 0
C7B 1 0.819604 0.308566 0.268200 11.00000 0.06932 0.09851 =
0.04556 0.02871 0.03311 0.03038
AFIX 137
H7B1 2 0.760709 0.335221 0.255780 11.00000 -1.50000
H7B2 2 0.849827 0.283800 0.239545 11.00000 -1.50000
H7B3 2 0.853230 0.368419 0.285943 11.00000 -1.50000
AFIX 0
C8B 1 0.703006 0.102296 0.242991 11.00000 0.06393 0.16579 =
0.02161 -0.01665 -0.00282 0.02153
AFIX 137
H8B1 2 0.663210 0.040028 0.246413 11.00000 -1.50000
H8B2 2 0.738886 0.087550 0.215354 11.00000 -1.50000
H8B3 2 0.668506 0.169598 0.235531 11.00000 -1.50000
AFIX 0
C9B 1 0.738350 -0.073009 0.331971 11.00000 0.05945 0.08215 =
0.05845 -0.01826 0.01840 0.00733
AFIX 137
H9B1 2 0.774753 -0.124745 0.315034 11.00000 -1.50000
H9B2 2 0.678582 -0.072468 0.314444 11.00000 -1.50000
H9B3 2 0.736486 -0.096048 0.367184 11.00000 -1.50000
AFIX 0
C10B 1 0.881175 0.032255 0.415089 11.00000 0.04668 0.09307 =
0.03412 0.01108 0.00633 0.02296
AFIX 137
H10A 2 0.903750 0.087715 0.440023 11.00000 -1.50000
H10B 2 0.929495 -0.015407 0.407028 11.00000 -1.50000
H10C 2 0.836250 -0.012513 0.429076 11.00000 -1.50000
AFIX 0
MOLE 2
B1C 3 0.069503 0.751776 0.882912 11.00000 0.04402 0.03887 =
0.02491 -0.00121 0.00928 0.00188
C11C 1 0.020326 0.748083 0.824151 11.00000 0.03419 0.04056 =
0.02383 -0.00201 0.01081 0.00234
C12C 1 0.016030 0.838787 0.791239 11.00000 0.03780 0.04552 =
0.02788 -0.00153 0.00905 -0.00151
AFIX 43
H12D 2 0.045315 0.904882 0.802481 11.00000 -1.20000
AFIX 0
C13C 1 -0.029233 0.836573 0.742744 11.00000 0.04306 0.05595 =
0.03050 0.00755 0.00702 0.00435
AFIX 43
H13D 2 -0.030115 0.900073 0.721738 11.00000 -1.20000
AFIX 0
C14C 1 -0.073141 0.740988 0.725200 11.00000 0.03810 0.06940 =
0.02674 -0.00417 0.00393 0.00221
AFIX 43
H14D 2 -0.104753 0.738687 0.692409 11.00000 -1.20000
AFIX 0
C15C 1 -0.069780 0.650001 0.756335 11.00000 0.04043 0.05495 =
0.03785 -0.01160 0.01084 -0.00436
AFIX 43
H15C 2 -0.099390 0.584283 0.744860 11.00000 -1.20000
AFIX 0
C16C 1 -0.023753 0.652978 0.804224 11.00000 0.04282 0.04251 =
0.03010 -0.00203 0.01251 0.00180
AFIX 43
H16C 2 -0.021850 0.588209 0.824448 11.00000 -1.20000
AFIX 0
C21C 1 0.108384 0.627362 0.897611 11.00000 0.03697 0.04220 =
0.02410 -0.00204 0.00392 0.00216
C22C 1 0.157289 0.567113 0.864871 11.00000 0.06313 0.05493 =
0.02804 0.00197 0.01234 0.01194
AFIX 43
H22C 2 0.170424 0.601676 0.834503 11.00000 -1.20000
AFIX 0
C23C 1 0.187195 0.460703 0.874425 11.00000 0.05722 0.05490 =
0.03984 -0.00675 0.00928 0.01462
AFIX 43
H23C 2 0.220496 0.424458 0.851182 11.00000 -1.20000
AFIX 0
C24C 1 0.168372 0.407053 0.918103 11.00000 0.05303 0.03921 =
0.04383 -0.00076 -0.00893 0.00316
AFIX 43
H24C 2 0.188073 0.333715 0.925014 11.00000 -1.20000
AFIX 0
C25C 1 0.120672 0.462096 0.951166 11.00000 0.04175 0.04977 =
0.02975 0.00473 -0.00414 -0.00230
AFIX 43
H25C 2 0.107037 0.426316 0.981145 11.00000 -1.20000
AFIX 0
C26C 1 0.092215 0.569443 0.941199 11.00000 0.03457 0.04133 =
0.02529 -0.00170 -0.00041 -0.00319
AFIX 43
H26C 2 0.060186 0.605355 0.965150 11.00000 -1.20000
AFIX 0
C31C 1 0.148626 0.844587 0.886604 11.00000 0.04796 0.04839 =
0.01665 0.00080 0.00564 -0.00207
C32C 1 0.237041 0.820228 0.886569 11.00000 0.05083 0.06988 =
0.02207 0.00516 0.00835 -0.00970
AFIX 43
H32C 2 0.254059 0.744912 0.885796 11.00000 -1.20000
AFIX 0
C33C 1 0.302741 0.901162 0.887617 11.00000 0.05688 0.09589 =
0.02981 0.00306 0.01263 -0.02283
AFIX 43
H33C 2 0.362535 0.880124 0.887474 11.00000 -1.20000
AFIX 0
C34C 1 0.280418 1.011530 0.888858 11.00000 0.08078 0.09116 =
0.02908 -0.00235 0.01155 -0.04894
AFIX 43
H34C 2 0.324337 1.067142 0.889839 11.00000 -1.20000
AFIX 0
C35C 1 0.192843 1.039114 0.888639 11.00000 0.09480 0.05605 =
0.02822 -0.00241 0.00659 -0.02586
AFIX 43
H35C 2 0.176400 1.114674 0.889030 11.00000 -1.20000
AFIX 0
C36C 1 0.128109 0.957993 0.887856 11.00000 0.06389 0.04977 =
0.02633 -0.00136 0.00202 -0.01199
AFIX 43
H36C 2 0.068494 0.979677 0.888174 11.00000 -1.20000
AFIX 0
C41C 1 -0.003793 0.782834 0.921777 11.00000 0.05529 0.03483 =
0.02737 0.00557 0.01397 0.00777
C42C 1 0.016158 0.841079 0.966686 11.00000 0.05860 0.04375 =
0.02644 -0.00060 0.00789 0.01054
AFIX 43
H42C 2 0.074376 0.867668 0.974915 11.00000 -1.20000
AFIX 0
C43C 1 -0.047056 0.862067 1.000463 11.00000 0.07823 0.04211 =
0.03031 -0.00148 0.01559 0.01609
AFIX 43
H43C 2 -0.031259 0.903498 1.030417 11.00000 -1.20000
AFIX 0
C44C 1 -0.130705 0.823039 0.990209 11.00000 0.08129 0.05662 =
0.03857 0.00922 0.03226 0.02041
AFIX 43
H44C 2 -0.173072 0.836511 1.013098 11.00000 -1.20000
AFIX 0
C45C 1 -0.153346 0.764069 0.946536 11.00000 0.06030 0.07619 =
0.05445 -0.00397 0.03122 -0.00338
AFIX 43
H45C 2 -0.211214 0.735624 0.939296 11.00000 -1.20000
AFIX 0
C46C 1 -0.090734 0.746265 0.912898 11.00000 0.05451 0.06113 =
0.03941 -0.00751 0.02219 -0.00227
AFIX 43
H46C 2 -0.108119 0.707316 0.882429 11.00000 -1.20000
HKLF 4
REM Marina7_P21byc in P2(1)/c
REM R1 = 0.0670 for 7228 Fo > 4sig(Fo) and 0.0784 for all 8609 data
REM 603 parameters refined using 4 restraints
END
WGHT 0.1060 15.6385
REM Highest difference peak 2.049, deepest hole -0.572, 1-sigma level 0.121
Q1 1 0.5696 0.1686 0.3186 11.00000 0.05 2.05
Q2 1 0.5770 0.2501 0.3209 11.00000 0.05 1.75
Q3 1 0.5594 0.4529 0.3071 11.00000 0.05 1.64
Q4 1 0.5370 0.4789 0.2545 11.00000 0.05 1.40
Q5 1 0.6030 0.5155 0.2264 11.00000 0.05 1.33
Q6 1 0.7088 0.5176 0.3014 11.00000 0.05 1.30
Q7 1 0.6841 0.5372 0.2488 11.00000 0.05 1.23
Q8 1 0.5814 0.5348 0.1691 11.00000 0.05 1.22
Q9 1 0.7280 0.2737 0.3597 11.00000 0.05 0.78
Q10 1 0.6385 0.4585 0.3228 11.00000 0.05 0.73
Q11 1 0.6534 0.4548 0.3716 11.00000 0.05 0.71
Q12 1 0.6462 0.5228 0.4135 11.00000 0.05 0.70
Q13 1 0.4726 0.4174 0.3360 11.00000 0.05 0.63
Q14 1 0.5435 0.4423 0.1583 11.00000 0.05 0.51
Q15 1 0.4993 0.3591 0.2077 11.00000 0.05 0.47
Q16 1 0.8140 0.5329 0.3215 11.00000 0.05 0.43
Q17 1 0.6962 0.3894 0.4420 11.00000 0.05 0.42
Q18 1 0.6704 0.4744 0.4595 11.00000 0.05 0.40
Q19 1 0.9244 0.3242 0.3850 11.00000 0.05 0.38
Q20 1 0.5553 0.3920 0.2029 11.00000 0.05 0.38
;
_database_code_depnum_ccdc_archive 'CCDC 934047'