Supplementary Material (ESI) for Dalton Transactions
This journal is © The Royal Society of Chemistry 2010
data_global
_journal_name_full 'Dalton Trans.'
_journal_coden_Cambridge 0222
_journal_volume ?
_journal_page_first ?
_journal_year ?
_publ_contact_author_name 'Lau, Tai-Chu'
_publ_contact_author_email bhtclau@cityu.edu.hk
_publ_section_title
;
Formation of \^I-Dinitrogen (Salen)Osmium
complexes via Ligand-induced NN Coupling
of (Salen)osmium(VI) Nitrides
;
_publ_author_name T.-C.Lau
# Attachment '- ALL.cif'
data_1b
_database_code_depnum_ccdc_archive 'CCDC 777079'
#TrackingRef '- ALL.cif'
# wt1200w-TCLau-BB31_25-2-2006
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C21 H24 N3 O3 Os, Cl O4'
_chemical_formula_sum 'C21 H24 Cl N3 O7 Os'
_chemical_formula_weight 656.08
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'
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'
Os Os -1.2165 7.6030 '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'
H H 0.0000 0.0000 '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'
_symmetry_Int_Tables_number 14
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 11.815(2)
_cell_length_b 15.116(2)
_cell_length_c 13.643(2)
_cell_angle_alpha 90.00
_cell_angle_beta 111.240(10)
_cell_angle_gamma 90.00
_cell_volume 2271.1(6)
_cell_formula_units_Z 4
_cell_measurement_temperature 299(2)
_cell_measurement_reflns_used 13856
_cell_measurement_theta_min 1.35
_cell_measurement_theta_max 27.51
_exptl_crystal_description block
_exptl_crystal_colour brown
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.16
_exptl_crystal_size_min 0.13
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.919
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1280
_exptl_absorpt_coefficient_mu 5.781
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.3910
_exptl_absorpt_correction_T_max 0.5203
_exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 299(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 SMART 1000 CCD'
_diffrn_measurement_method \w
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number 0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time .
_diffrn_standards_decay_% ?
_diffrn_reflns_number 5072
_diffrn_reflns_av_R_equivalents 0.0228
_diffrn_reflns_av_sigmaI/netI 0.0317
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_theta_min 1.96
_diffrn_reflns_theta_max 27.51
_reflns_number_total 5072
_reflns_number_gt 4061
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'SMART (Bruker AXS Inc., 1998)'
_computing_cell_refinement 'SAINT (Bruker AXS Inc.,1999)'
_computing_data_reduction
'SAINT & CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2006)'
_computing_structure_solution 'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'ORTEP-II (Johnson, 1976) & Mercury'
_computing_publication_material SHELXL-97
_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^)+(0.0136P)^2^] 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 5072
_refine_ls_number_parameters 385
_refine_ls_number_restraints 53
_refine_ls_R_factor_all 0.0293
_refine_ls_R_factor_gt 0.0205
_refine_ls_wR_factor_ref 0.0419
_refine_ls_wR_factor_gt 0.0409
_refine_ls_goodness_of_fit_ref 1.059
_refine_ls_restrained_S_all 1.076
_refine_ls_shift/su_max 0.028
_refine_ls_shift/su_mean 0.001
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
Os1 Os 0.300759(11) 0.543639(9) 0.556758(9) 0.03322(4) Uani 1 1 d . . .
O1 O 0.29201(19) 0.53159(16) 0.41004(16) 0.0417(6) Uani 1 1 d . C .
O2 O 0.45889(19) 0.60171(16) 0.57614(17) 0.0405(6) Uani 1 1 d . C .
O3 O 0.4279(2) 0.41714(17) 0.56777(18) 0.0452(6) Uani 1 1 d . C .
H3O H 0.4566 0.4247 0.5125 0.054 Uiso 1 1 d . . .
Cl1 Cl 0.15699(11) 0.15402(7) 0.47871(9) 0.0632(3) Uani 0.668(10) 1 d PD A 1
O4 O 0.0391(5) 0.1961(5) 0.4401(8) 0.130(4) Uani 0.668(10) 1 d PD A 1
O5 O 0.1972(8) 0.1555(5) 0.5913(4) 0.116(3) Uani 0.668(10) 1 d PD A 1
O6 O 0.2316(8) 0.2049(8) 0.4536(10) 0.192(6) Uani 0.668(10) 1 d PD A 1
O7 O 0.1434(12) 0.0684(5) 0.4461(8) 0.163(5) Uani 0.668(10) 1 d PDU A 1
Cl1B Cl 0.15699(11) 0.15402(7) 0.47871(9) 0.0632(3) Uani 0.332(10) 1 d PD A 2
O4B O 0.0955(18) 0.2047(10) 0.3889(10) 0.126(7) Uani 0.332(10) 1 d PDU A 2
O5B O 0.0789(13) 0.1151(14) 0.5136(15) 0.147(8) Uani 0.332(10) 1 d PDU A 2
O6B O 0.2347(13) 0.2069(11) 0.5454(15) 0.127(6) Uani 0.332(10) 1 d PDU A 2
O7B O 0.2310(17) 0.0917(13) 0.4549(13) 0.139(9) Uani 0.332(10) 1 d PD A 2
N3 N 0.2116(3) 0.6265(2) 0.5536(2) 0.0493(7) Uani 1 1 d . C .
C1 C 0.2001(3) 0.4903(2) 0.3341(3) 0.0386(8) Uani 1 1 d . . .
C2 C 0.1911(3) 0.5060(3) 0.2309(3) 0.0464(9) Uani 1 1 d . C .
H2 H 0.2455 0.5445 0.2179 0.056 Uiso 1 1 calc R . .
C3 C 0.1028(4) 0.4653(3) 0.1480(3) 0.0572(10) Uani 1 1 d . . .
H3 H 0.0983 0.4766 0.0797 0.069 Uiso 1 1 calc R C .
C4 C 0.0206(4) 0.4079(3) 0.1648(3) 0.0598(11) Uani 1 1 d . C .
H4 H -0.0392 0.3812 0.1081 0.072 Uiso 1 1 calc R . .
C5 C 0.0278(3) 0.3907(3) 0.2651(3) 0.0519(10) Uani 1 1 d . . .
H5 H -0.0269 0.3513 0.2761 0.062 Uiso 1 1 calc R C .
C6 C 0.1170(3) 0.4317(2) 0.3530(3) 0.0406(8) Uani 1 1 d . C .
C7 C 0.1170(3) 0.4075(2) 0.4545(3) 0.0404(8) Uani 1 1 d . . .
H7 H 0.0658 0.3615 0.4570 0.048 Uiso 1 1 calc R B 1
N1 N 0.1816(2) 0.44376(19) 0.5433(2) 0.0373(6) Uani 0.677(11) 1 d PD C 1
C8 C 0.1961(6) 0.3988(5) 0.6433(5) 0.0363(15) Uani 0.677(11) 1 d PD C 1
H8 H 0.2563 0.3516 0.6540 0.044 Uiso 0.677(11) 1 calc PR C 1
C9 C 0.0808(16) 0.3574(12) 0.6480(11) 0.0452(16) Uani 0.677(11) 1 d PD C 1
H9A H 0.0501 0.3133 0.5931 0.054 Uiso 0.677(11) 1 calc PR C 1
H9B H 0.0190 0.4025 0.6371 0.054 Uiso 0.677(11) 1 calc PR C 1
C10 C 0.1105(9) 0.3142(6) 0.7566(7) 0.058(2) Uani 0.677(11) 1 d PD C 1
H10A H 0.0356 0.2936 0.7628 0.070 Uiso 0.677(11) 1 calc PR C 1
H10B H 0.1618 0.2630 0.7614 0.070 Uiso 0.677(11) 1 calc PR C 1
C11 C 0.1731(16) 0.3750(14) 0.8462(9) 0.061(4) Uani 0.677(11) 1 d PD C 1
H11A H 0.1157 0.4194 0.8503 0.073 Uiso 0.677(11) 1 calc PR C 1
H11B H 0.1989 0.3414 0.9112 0.073 Uiso 0.677(11) 1 calc PR C 1
C12 C 0.2811(15) 0.4204(12) 0.8367(12) 0.054(4) Uani 0.677(11) 1 d PD C 1
H12A H 0.3444 0.3772 0.8439 0.065 Uiso 0.677(11) 1 calc PR C 1
H12B H 0.3124 0.4634 0.8928 0.065 Uiso 0.677(11) 1 calc PR C 1
C13 C 0.2475(6) 0.4662(5) 0.7319(5) 0.0377(16) Uani 0.677(11) 1 d PD C 1
H13 H 0.1834 0.5092 0.7265 0.045 Uiso 0.677(11) 1 calc PR C 1
N2 N 0.3492(2) 0.51464(19) 0.7114(2) 0.0375(6) Uani 0.677(11) 1 d PD C 1
N1B N 0.1816(2) 0.44376(19) 0.5433(2) 0.0373(6) Uani 0.323(11) 1 d PD C 2
C8B C 0.1629(10) 0.4334(10) 0.6485(8) 0.032(3) Uani 0.323(11) 1 d PD C 2
H8B H 0.1194 0.4862 0.6573 0.038 Uiso 0.323(11) 1 calc PR C 2
C9B C 0.091(4) 0.355(2) 0.661(2) 0.0452(16) Uani 0.323(11) 1 d PD C 2
H9B1 H 0.0106 0.3571 0.6070 0.054 Uiso 0.323(11) 1 calc PR C 2
H9B2 H 0.1304 0.3012 0.6507 0.054 Uiso 0.323(11) 1 calc PR C 2
C10B C 0.0808(16) 0.3528(12) 0.7666(14) 0.049(4) Uani 0.323(11) 1 d PD C 2
H10C H 0.0433 0.2975 0.7743 0.058 Uiso 0.323(11) 1 calc PR C 2
H10D H 0.0280 0.4005 0.7711 0.058 Uiso 0.323(11) 1 calc PR C 2
C11B C 0.201(3) 0.362(3) 0.855(2) 0.077(14) Uani 0.323(11) 1 d PD C 2
H11C H 0.2462 0.3072 0.8606 0.092 Uiso 0.323(11) 1 calc PR C 2
H11D H 0.1864 0.3688 0.9205 0.092 Uiso 0.323(11) 1 calc PR C 2
C12B C 0.280(3) 0.439(2) 0.844(2) 0.034(5) Uani 0.323(11) 1 d PD C 2
H12C H 0.2435 0.4949 0.8533 0.040 Uiso 0.323(11) 1 calc PR C 2
H12D H 0.3601 0.4353 0.8982 0.040 Uiso 0.323(11) 1 calc PR C 2
C13B C 0.2878(11) 0.4353(10) 0.7361(10) 0.037(3) Uani 0.323(11) 1 d PD C 2
H13B H 0.3327 0.3820 0.7314 0.044 Uiso 0.323(11) 1 calc PR C 2
N2B N 0.3492(2) 0.51464(19) 0.7114(2) 0.0375(6) Uani 0.323(11) 1 d PD C 2
C14 C 0.4438(3) 0.5476(2) 0.7843(2) 0.0408(7) Uani 1 1 d . . .
H14 H 0.4575 0.5306 0.8532 0.049 Uiso 1 1 calc R C 1
C15 C 0.5294(3) 0.6082(2) 0.7683(3) 0.0374(7) Uani 1 1 d . C .
C16 C 0.6138(3) 0.6458(3) 0.8592(3) 0.0491(9) Uani 1 1 d . . .
H16 H 0.6121 0.6296 0.9245 0.059 Uiso 1 1 calc R C .
C17 C 0.6991(3) 0.7060(3) 0.8550(3) 0.0537(10) Uani 1 1 d . C .
H17 H 0.7526 0.7317 0.9161 0.064 Uiso 1 1 calc R . .
C18 C 0.7039(3) 0.7274(3) 0.7580(3) 0.0487(9) Uani 1 1 d . . .
H18 H 0.7627 0.7667 0.7543 0.058 Uiso 1 1 calc R C .
C19 C 0.6230(3) 0.6914(2) 0.6666(3) 0.0408(8) Uani 1 1 d . C .
H19 H 0.6276 0.7069 0.6022 0.049 Uiso 1 1 calc R . .
C20 C 0.5349(3) 0.6324(2) 0.6701(2) 0.0346(7) Uani 1 1 d . . .
C21 C 0.4906(4) 0.3534(3) 0.6417(4) 0.0746(14) Uani 1 1 d . . .
H21A H 0.5647 0.3384 0.6319 0.089 Uiso 1 1 calc R C .
H21B H 0.4411 0.3015 0.6328 0.089 Uiso 1 1 calc R . .
H21C H 0.5089 0.3766 0.7113 0.089 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
Os1 0.03201(6) 0.03415(7) 0.03207(6) 0.00073(7) 0.00989(4) -0.00316(7)
O1 0.0388(12) 0.0524(16) 0.0318(11) 0.0025(11) 0.0103(9) -0.0054(11)
O2 0.0389(12) 0.0480(15) 0.0357(12) -0.0055(11) 0.0149(10) -0.0148(11)
O3 0.0465(13) 0.0481(15) 0.0474(14) 0.0078(12) 0.0247(11) 0.0094(11)
Cl1 0.0773(7) 0.0508(6) 0.0694(7) -0.0032(5) 0.0361(6) -0.0089(5)
O4 0.075(4) 0.115(7) 0.179(9) -0.024(6) 0.023(5) -0.003(4)
O5 0.182(8) 0.103(6) 0.077(4) -0.005(4) 0.061(5) 0.010(5)
O6 0.144(8) 0.232(13) 0.233(12) 0.107(10) 0.108(9) -0.043(7)
O7 0.237(11) 0.062(4) 0.136(7) -0.028(4) 0.003(8) 0.002(6)
Cl1B 0.0773(7) 0.0508(6) 0.0694(7) -0.0032(5) 0.0361(6) -0.0089(5)
O4B 0.153(14) 0.109(10) 0.092(9) 0.057(8) 0.015(8) 0.021(10)
O5B 0.106(10) 0.183(15) 0.186(15) 0.071(12) 0.092(10) -0.015(9)
O6B 0.096(8) 0.105(9) 0.143(10) -0.049(8) 0.002(7) 0.006(7)
O7B 0.150(15) 0.17(2) 0.117(12) -0.074(12) 0.066(12) 0.053(13)
N3 0.0541(17) 0.0442(19) 0.0510(18) 0.0006(16) 0.0207(15) -0.0006(15)
C1 0.0379(18) 0.0357(19) 0.0362(18) 0.0004(15) 0.0065(14) 0.0082(15)
C2 0.050(2) 0.049(2) 0.0382(19) 0.0049(17) 0.0135(16) 0.0028(17)
C3 0.065(2) 0.064(3) 0.0351(18) -0.002(2) 0.0087(17) 0.008(2)
C4 0.055(2) 0.063(3) 0.047(2) -0.013(2) 0.0003(19) -0.001(2)
C5 0.043(2) 0.054(3) 0.052(2) -0.0120(19) 0.0081(17) -0.0058(18)
C6 0.0374(17) 0.041(2) 0.0388(18) -0.0024(15) 0.0087(15) 0.0015(14)
C7 0.0346(17) 0.038(2) 0.045(2) -0.0017(16) 0.0102(15) -0.0037(15)
N1 0.0298(13) 0.0431(18) 0.0376(14) 0.0010(13) 0.0103(11) -0.0025(12)
C8 0.033(3) 0.036(4) 0.042(3) 0.000(3) 0.016(3) 0.001(3)
C9 0.042(4) 0.050(2) 0.043(4) -0.002(3) 0.014(4) -0.012(2)
C10 0.058(5) 0.066(7) 0.057(4) 0.001(5) 0.028(4) -0.024(4)
C11 0.071(8) 0.073(7) 0.049(7) 0.006(6) 0.035(6) -0.023(6)
C12 0.064(6) 0.057(9) 0.037(5) -0.002(5) 0.014(5) -0.015(5)
C13 0.034(4) 0.042(4) 0.042(3) 0.000(3) 0.020(3) -0.004(3)
N2 0.0397(15) 0.0399(17) 0.0346(14) -0.0021(12) 0.0153(12) -0.0080(12)
N1B 0.0298(13) 0.0431(18) 0.0376(14) 0.0010(13) 0.0103(11) -0.0025(12)
C8B 0.031(6) 0.040(9) 0.025(5) 0.001(5) 0.011(5) 0.003(5)
C9B 0.042(4) 0.050(2) 0.043(4) -0.002(3) 0.014(4) -0.012(2)
C10B 0.056(10) 0.052(11) 0.046(8) -0.004(8) 0.028(7) -0.019(8)
C11B 0.068(17) 0.09(2) 0.050(13) 0.017(13) -0.005(11) -0.029(16)
C12B 0.036(9) 0.035(10) 0.035(9) -0.003(7) 0.019(7) -0.020(7)
C13B 0.031(7) 0.038(8) 0.043(7) 0.003(6) 0.016(6) 0.001(5)
N2B 0.0397(15) 0.0399(17) 0.0346(14) -0.0021(12) 0.0153(12) -0.0080(12)
C14 0.0455(18) 0.046(2) 0.0312(16) -0.0008(17) 0.0137(14) -0.0040(17)
C15 0.0344(16) 0.0372(19) 0.0359(17) -0.0032(15) 0.0071(14) -0.0035(14)
C16 0.048(2) 0.056(3) 0.0376(19) -0.0012(18) 0.0081(16) -0.0094(18)
C17 0.044(2) 0.057(3) 0.047(2) -0.0077(19) 0.0016(17) -0.0131(18)
C18 0.0380(18) 0.046(2) 0.060(2) -0.0057(19) 0.0147(17) -0.0111(16)
C19 0.0401(18) 0.041(2) 0.0438(19) -0.0034(16) 0.0178(15) -0.0066(15)
C20 0.0304(15) 0.0333(18) 0.0382(17) -0.0035(15) 0.0104(13) 0.0016(14)
C21 0.067(3) 0.075(3) 0.093(3) 0.041(3) 0.043(3) 0.032(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
Os1 N3 1.627(3) . ?
Os1 O1 1.975(2) . ?
Os1 O2 1.993(2) . ?
Os1 N2 2.024(3) . ?
Os1 N1 2.027(3) . ?
Os1 O3 2.403(2) . ?
O1 C1 1.352(4) . ?
O2 C20 1.352(4) . ?
O3 C21 1.397(4) . ?
O3 H3O 0.9395 . ?
Cl1 O6 1.306(6) . ?
Cl1 O7 1.359(7) . ?
Cl1 O5 1.434(6) . ?
Cl1 O4 1.446(6) . ?
C1 C2 1.393(5) . ?
C1 C6 1.414(5) . ?
C2 C3 1.375(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.382(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.366(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.420(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.432(5) . ?
C7 N1 1.296(4) . ?
C7 H7 0.9300 . ?
N1 C8 1.478(7) . ?
C8 C9 1.520(15) . ?
C8 C13 1.529(8) . ?
C8 H8 0.9800 . ?
C9 C10 1.539(16) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.494(13) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.494(17) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.506(16) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 N2 1.517(6) . ?
C13 H13 0.9800 . ?
N2 C14 1.297(4) . ?
C8B C9B 1.50(2) . ?
C8B C13B 1.527(13) . ?
C8B H8B 0.9800 . ?
C9B C10B 1.49(3) . ?
C9B H9B1 0.9700 . ?
C9B H9B2 0.9700 . ?
C10B C11B 1.501(19) . ?
C10B H10C 0.9700 . ?
C10B H10D 0.9700 . ?
C11B C12B 1.54(3) . ?
C11B H11C 0.9700 . ?
C11B H11D 0.9700 . ?
C12B C13B 1.52(2) . ?
C12B H12C 0.9700 . ?
C12B H12D 0.9700 . ?
C13B H13B 0.9800 . ?
C14 C15 1.438(4) . ?
C14 H14 0.9300 . ?
C15 C16 1.401(4) . ?
C15 C20 1.413(4) . ?
C16 C17 1.374(5) . ?
C16 H16 0.9300 . ?
C17 C18 1.383(5) . ?
C17 H17 0.9300 . ?
C18 C19 1.378(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.385(4) . ?
C19 H19 0.9300 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
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
N3 Os1 O1 104.39(12) . . ?
N3 Os1 O2 103.37(13) . . ?
O1 Os1 O2 82.96(9) . . ?
N3 Os1 N2 97.47(13) . . ?
O1 Os1 N2 158.09(11) . . ?
O2 Os1 N2 93.42(10) . . ?
N3 Os1 N1 98.57(13) . . ?
O1 Os1 N1 93.44(10) . . ?
O2 Os1 N1 157.98(10) . . ?
N2 Os1 N1 81.83(10) . . ?
N3 Os1 O3 176.83(12) . . ?
O1 Os1 O3 77.99(9) . . ?
O2 Os1 O3 78.89(9) . . ?
N2 Os1 O3 80.11(10) . . ?
N1 Os1 O3 79.11(10) . . ?
C1 O1 Os1 123.5(2) . . ?
C20 O2 Os1 123.03(19) . . ?
C21 O3 Os1 138.5(2) . . ?
C21 O3 H3O 114.4 . . ?
Os1 O3 H3O 104.7 . . ?
O6 Cl1 O7 119.1(8) . . ?
O6 Cl1 O5 106.2(6) . . ?
O7 Cl1 O5 108.7(5) . . ?
O6 Cl1 O4 107.3(6) . . ?
O7 Cl1 O4 108.4(6) . . ?
O5 Cl1 O4 106.6(5) . . ?
O1 C1 C2 116.2(3) . . ?
O1 C1 C6 124.6(3) . . ?
C2 C1 C6 119.2(3) . . ?
C3 C2 C1 120.8(4) . . ?
C3 C2 H2 119.6 . . ?
C1 C2 H2 119.6 . . ?
C2 C3 C4 120.9(4) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
C5 C4 C3 119.6(4) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 121.4(4) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C1 C6 C5 118.1(3) . . ?
C1 C6 C7 125.4(3) . . ?
C5 C6 C7 116.4(3) . . ?
N1 C7 C6 126.1(3) . . ?
N1 C7 H7 116.9 . . ?
C6 C7 H7 116.9 . . ?
C7 N1 C8 120.0(4) . . ?
C7 N1 Os1 123.6(2) . . ?
C8 N1 Os1 114.5(3) . . ?
N1 C8 C9 115.0(8) . . ?
N1 C8 C13 107.7(5) . . ?
C9 C8 C13 110.3(8) . . ?
N1 C8 H8 107.9 . . ?
C9 C8 H8 107.9 . . ?
C13 C8 H8 107.9 . . ?
C8 C9 C10 108.7(11) . . ?
C8 C9 H9A 110.0 . . ?
C10 C9 H9A 110.0 . . ?
C8 C9 H9B 110.0 . . ?
C10 C9 H9B 110.0 . . ?
H9A C9 H9B 108.3 . . ?
C11 C10 C9 113.5(11) . . ?
C11 C10 H10A 108.9 . . ?
C9 C10 H10A 108.9 . . ?
C11 C10 H10B 108.9 . . ?
C9 C10 H10B 108.9 . . ?
H10A C10 H10B 107.7 . . ?
C12 C11 C10 113.4(13) . . ?
C12 C11 H11A 108.9 . . ?
C10 C11 H11A 108.9 . . ?
C12 C11 H11B 108.9 . . ?
C10 C11 H11B 108.9 . . ?
H11A C11 H11B 107.7 . . ?
C11 C12 C13 110.7(12) . . ?
C11 C12 H12A 109.5 . . ?
C13 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C13 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
C12 C13 N2 116.3(7) . . ?
C12 C13 C8 109.7(9) . . ?
N2 C13 C8 106.9(5) . . ?
C12 C13 H13 107.9 . . ?
N2 C13 H13 107.9 . . ?
C8 C13 H13 107.9 . . ?
C14 N2 C13 124.3(3) . . ?
C14 N2 Os1 123.8(2) . . ?
C13 N2 Os1 110.7(3) . . ?
C9B C8B C13B 110.7(18) . . ?
C9B C8B H8B 106.8 . . ?
C13B C8B H8B 106.8 . . ?
C10B C9B C8B 111.9(19) . . ?
C10B C9B H9B1 109.2 . . ?
C8B C9B H9B1 109.2 . . ?
C10B C9B H9B2 109.2 . . ?
C8B C9B H9B2 109.2 . . ?
H9B1 C9B H9B2 107.9 . . ?
C9B C10B C11B 113(2) . . ?
C9B C10B H10C 109.0 . . ?
C11B C10B H10C 109.0 . . ?
C9B C10B H10D 109.0 . . ?
C11B C10B H10D 109.0 . . ?
H10C C10B H10D 107.8 . . ?
C10B C11B C12B 115(2) . . ?
C10B C11B H11C 108.6 . . ?
C12B C11B H11C 108.6 . . ?
C10B C11B H11D 108.6 . . ?
C12B C11B H11D 108.6 . . ?
H11C C11B H11D 107.6 . . ?
C13B C12B C11B 109(2) . . ?
C13B C12B H12C 110.0 . . ?
C11B C12B H12C 110.0 . . ?
C13B C12B H12D 110.0 . . ?
C11B C12B H12D 110.0 . . ?
H12C C12B H12D 108.4 . . ?
C12B C13B C8B 112.2(15) . . ?
C12B C13B H13B 109.0 . . ?
C8B C13B H13B 109.0 . . ?
N2 C14 C15 125.9(3) . . ?
N2 C14 H14 117.1 . . ?
C15 C14 H14 117.1 . . ?
C16 C15 C20 118.2(3) . . ?
C16 C15 C14 116.0(3) . . ?
C20 C15 C14 125.9(3) . . ?
C17 C16 C15 121.9(3) . . ?
C17 C16 H16 119.0 . . ?
C15 C16 H16 119.0 . . ?
C16 C17 C18 118.7(3) . . ?
C16 C17 H17 120.7 . . ?
C18 C17 H17 120.7 . . ?
C19 C18 C17 121.2(3) . . ?
C19 C18 H18 119.4 . . ?
C17 C18 H18 119.4 . . ?
C18 C19 C20 120.5(3) . . ?
C18 C19 H19 119.8 . . ?
C20 C19 H19 119.8 . . ?
O2 C20 C19 116.0(3) . . ?
O2 C20 C15 124.5(3) . . ?
C19 C20 C15 119.5(3) . . ?
O3 C21 H21A 109.5 . . ?
O3 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O3 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3O O2 0.94 1.868 2.762(3) 157.9 3_666
loop_
_publ_manuscript_incl_extra_item
I
J
CgI...CgJ
'Dihedral angle'
CgI_Perp
CgJ_Perp
C--H
CgJ
H...CgJ
C-H...CgJ
C...CgJ
loop_
_geom_extra_tableA_col_1
_geom_extra_tableA_col_2
_geom_extra_tableA_col_3
_geom_extra_tableA_col_4
_geom_extra_tableA_col_5
_geom_extra_tableA_col_6
I J CgI...CgJ 'Dihedral angle' CgI_Perp
CgJ_Perp
1 2^i^ 3.733(2) 0.90(19) -3.4646(17) -3.4559(16)
2 1^i^ 3.733(2) 0.90(19) -3.4558(16) -3.4646(17)
_geom_extra_table_head_A
;
Table 1. \p...\p interactions (\%A, \%)
Cg1 and Cg2 are centroids of the rings C1-C6 and C15-C20
respectively, CgI...CgJ is the distance between ring centroids.
The dihedral angle is that between the planes of the rings I
and J. CgI_Perp is the perpendicular distance of CgI
from ring J. CgJ_Perp is the perpendicular distance of
CgJ from ring I.
;
_geom_table_footnote_A
;
symmetry operators:
^i^: 1-X, 1-Y, 1-Z
;
loop_
_geom_extra_tableB_col_1
_geom_extra_tableB_col_2
_geom_extra_tableB_col_3
_geom_extra_tableB_col_4
_geom_extra_tableB_col_5
C--H CgJ H...CgJ C--H...CgJ C...CgJ
C10-H10A 2^ii^ 2.55 148 3.413(10)
C10B-H10C 2^ii^ 2.64 160 3.567(19)
C10B-H10D 1^iii^ 2.76 168 3.712(19)
_geom_extra_table_head_B
;
Table 2. C--H...\p interactions (\%A, \%)
Cg1 and Cg2 are centroids of the rings C1-C6 and
C15-C20 respectively, H...CgJ and 'C...CgJ' are
the distances between ring centroid and the specified atom H
and C respectively. C--H...CgJ is the angle between the
C--H bond and the ring centroid CgJ.
;
_geom_table_footnote_B
;
symmetry operators:
^ii^: 1/2-X,-1/2+Y,3/2-Z
^iii^: -X,1-Y,1-Z
;
_diffrn_measured_fraction_theta_max 0.970
_diffrn_reflns_theta_full 27.51
_diffrn_measured_fraction_theta_full 0.970
_refine_diff_density_max 0.984
_refine_diff_density_min -0.531
_refine_diff_density_rms 0.079
#==============================================================================
data_3
_database_code_depnum_ccdc_archive 'CCDC 777080'
#TrackingRef '- ALL.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C54 H57 F6 N9 O4 Os2 P'
_chemical_formula_weight 1421.46
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -4.9801 6.2216 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 11.6924(6)
_cell_length_b 15.9584(5)
_cell_length_c 16.5889(7)
_cell_angle_alpha 80.151(3)
_cell_angle_beta 86.130(4)
_cell_angle_gamma 89.368(3)
_cell_volume 3042.8(2)
_cell_formula_units_Z 2
_cell_measurement_temperature 173(2)
_cell_measurement_reflns_used 20781
_cell_measurement_theta_min 3.5537
_cell_measurement_theta_max 71.2798
_exptl_crystal_description needle
_exptl_crystal_colour 'dark red'
_exptl_crystal_size_max 0.6
_exptl_crystal_size_mid 0.11
_exptl_crystal_size_min 0.09
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.551
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1394
_exptl_absorpt_coefficient_mu 8.580
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.34111
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_process_details 'CrysAlisPro, Oxford Diffraction Ltd'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 173(2)
_diffrn_radiation_wavelength 1.54184
_diffrn_radiation_type CuK\a
_diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_monochromator mirror
_diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean 16.1270
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 28191
_diffrn_reflns_av_R_equivalents 0.0258
_diffrn_reflns_av_sigmaI/netI 0.0249
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_theta_min 3.56
_diffrn_reflns_theta_max 67.00
_reflns_number_total 10801
_reflns_number_gt 9361
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'CrysAlisPro, Oxford Diffraction Ltd'
_computing_cell_refinement 'CrysAlisPro, Oxford Diffraction Ltd'
_computing_data_reduction 'CrysAlisPro, Oxford Diffraction Ltd'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics Ortep-3
_computing_publication_material Wingx
_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.
Since some of the solvent molecules cannot be unambiguously identified
and appear with uncertainty, therefore their electron density have been
smoothed away using PLATON SQUEEZE. The squeeze results have been appended
to the last paragraph of the cif.
The disorder of PF6 counterion has been fixed by split model. Displacement
parameter restraint (ISOR) and distance restraint (DFIX) have been applied
to make the ADPs and bond distances of those badly behaved ellipsoids
arriving at more appropriate values.ISOR restraint has also been applied
to the disordered methyl group on the pyridine ligand.
;
_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^)+(0.0378P)^2^+17.3593P] 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 10801
_refine_ls_number_parameters 761
_refine_ls_number_restraints 132
_refine_ls_R_factor_all 0.0448
_refine_ls_R_factor_gt 0.0389
_refine_ls_wR_factor_ref 0.1009
_refine_ls_wR_factor_gt 0.0991
_refine_ls_goodness_of_fit_ref 1.120
_refine_ls_restrained_S_all 1.134
_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
Os1 Os -0.04547(2) 0.839245(15) 0.138962(14) 0.02506(8) Uani 1 1 d . . .
Os2 Os 0.04158(2) 0.836832(16) 0.425198(15) 0.02708(8) Uani 1 1 d . . .
P1A P 0.7095(8) 0.4434(5) 0.8057(5) 0.0617(18) Uani 0.65 1 d PDU A 1
F1A F 0.7551(8) 0.3549(6) 0.7866(6) 0.078(3) Uani 0.65 1 d PDU A 1
F2A F 0.8374(10) 0.4689(10) 0.8111(11) 0.196(7) Uani 0.65 1 d PDU A 1
F3A F 0.7167(14) 0.4833(8) 0.7131(6) 0.146(5) Uani 0.65 1 d PDU A 1
F4A F 0.5840(9) 0.4176(9) 0.7993(10) 0.154(5) Uani 0.65 1 d PDU A 1
F5A F 0.7000(13) 0.4051(9) 0.8998(6) 0.140(5) Uani 0.65 1 d PDU A 1
F6A F 0.6752(11) 0.5342(6) 0.8230(7) 0.111(4) Uani 0.65 1 d PDU A 1
P1B P 0.6810(13) 0.4471(10) 0.8109(10) 0.075(5) Uani 0.35 1 d PDU B 2
F1B F 0.7739(18) 0.3829(16) 0.7805(15) 0.21(2) Uani 0.35 1 d PDU B 2
F2B F 0.7594(19) 0.5236(14) 0.7701(15) 0.183(13) Uani 0.35 1 d PDU B 2
F3B F 0.6264(15) 0.4513(10) 0.7263(8) 0.081(5) Uani 0.35 1 d PDU B 2
F4B F 0.6027(14) 0.3714(9) 0.8502(11) 0.096(6) Uani 0.35 1 d PDU B 2
F5B F 0.7491(17) 0.4410(14) 0.8902(11) 0.115(8) Uani 0.35 1 d PDU B 2
F6B F 0.5891(16) 0.5087(10) 0.8399(10) 0.097(6) Uani 0.35 1 d PDU B 2
O1 O -0.0922(4) 0.8311(3) 0.0250(2) 0.0338(10) Uani 1 1 d . . .
O2 O 0.0823(4) 0.8344(3) 0.5419(2) 0.0334(9) Uani 1 1 d . . .
O3 O -0.1993(3) 0.8975(3) 0.1578(3) 0.0348(10) Uani 1 1 d . . .
O4 O 0.1998(3) 0.8891(3) 0.3887(3) 0.0361(10) Uani 1 1 d . . .
N1 N -0.0079(4) 0.8385(3) 0.2484(3) 0.0257(10) Uani 1 1 d . . .
N2 N 0.0109(4) 0.8353(3) 0.3152(3) 0.0265(10) Uani 1 1 d . . .
N3 N 0.0401(4) 0.9501(3) 0.1078(3) 0.0265(10) Uani 1 1 d . . .
N4 N 0.1089(4) 0.7951(3) 0.1002(3) 0.0291(11) Uani 1 1 d . . .
N5 N -0.1307(4) 0.7236(3) 0.1781(3) 0.0325(11) Uani 1 1 d . . .
N6 N -0.0394(4) 0.9514(3) 0.4094(3) 0.0254(10) Uani 1 1 d . . .
N7 N -0.1158(4) 0.7997(3) 0.4748(3) 0.0328(11) Uani 1 1 d . . .
N8 N 0.1168(5) 0.7157(3) 0.4389(3) 0.0399(13) Uani 1 1 d . C .
C1 C -0.2083(5) 0.9799(4) 0.1585(4) 0.0308(13) Uani 1 1 d . . .
C2 C -0.3210(5) 1.0109(5) 0.1727(4) 0.0384(15) Uani 1 1 d . . .
H2 H -0.3840 0.9725 0.1809 0.046 Uiso 1 1 calc R . .
C3 C -0.3398(6) 1.0954(5) 0.1747(5) 0.0464(17) Uani 1 1 d . . .
H3 H -0.4162 1.1149 0.1823 0.056 Uiso 1 1 calc R . .
C4 C -0.2512(6) 1.1531(5) 0.1659(5) 0.0460(17) Uani 1 1 d . . .
H4 H -0.2656 1.2111 0.1697 0.055 Uiso 1 1 calc R . .
C5 C -0.1411(6) 1.1248(4) 0.1515(4) 0.0372(14) Uani 1 1 d . . .
H5 H -0.0795 1.1642 0.1457 0.045 Uiso 1 1 calc R . .
C6 C -0.1168(5) 1.0393(4) 0.1451(4) 0.0296(13) Uani 1 1 d . . .
C7 C 0.0004(5) 1.0223(4) 0.1204(3) 0.0298(13) Uani 1 1 d . . .
H7 H 0.0528 1.0685 0.1128 0.036 Uiso 1 1 calc R . .
C8 C 0.1636(5) 0.9410(4) 0.0787(4) 0.0273(12) Uani 1 1 d . . .
H8 H 0.1662 0.9443 0.0179 0.033 Uiso 1 1 calc R . .
C9 C 0.2456(5) 1.0081(4) 0.0961(4) 0.0330(13) Uani 1 1 d . . .
H9A H 0.2419 1.0090 0.1557 0.040 Uiso 1 1 calc R . .
H9B H 0.2225 1.0649 0.0678 0.040 Uiso 1 1 calc R . .
C10 C 0.3686(5) 0.9887(4) 0.0664(4) 0.0384(15) Uani 1 1 d . . .
H10A H 0.3742 0.9959 0.0058 0.046 Uiso 1 1 calc R . .
H10B H 0.4216 1.0300 0.0825 0.046 Uiso 1 1 calc R . .
C11 C 0.4050(6) 0.8995(5) 0.1015(5) 0.0451(17) Uani 1 1 d . . .
H11A H 0.4062 0.8936 0.1619 0.054 Uiso 1 1 calc R . .
H11B H 0.4836 0.8890 0.0793 0.054 Uiso 1 1 calc R . .
C12 C 0.3228(5) 0.8334(4) 0.0803(4) 0.0402(15) Uani 1 1 d . . .
H12A H 0.3229 0.8376 0.0200 0.048 Uiso 1 1 calc R . .
H12B H 0.3475 0.7754 0.1039 0.048 Uiso 1 1 calc R . .
C13 C 0.2025(5) 0.8508(4) 0.1157(4) 0.0291(12) Uani 1 1 d . . .
H13 H 0.2050 0.8473 0.1763 0.035 Uiso 1 1 calc R . .
C14 C 0.1230(6) 0.7422(4) 0.0498(4) 0.0354(14) Uani 1 1 d . . .
H14 H 0.1985 0.7238 0.0367 0.043 Uiso 1 1 calc R . .
C15 C 0.0292(6) 0.7098(4) 0.0127(4) 0.0394(15) Uani 1 1 d . . .
C16 C 0.0430(7) 0.6332(5) -0.0184(5) 0.0490(18) Uani 1 1 d . . .
H16 H 0.1108 0.6007 -0.0088 0.059 Uiso 1 1 calc R . .
C17 C -0.0395(9) 0.6049(5) -0.0621(5) 0.059(2) Uani 1 1 d . . .
H17 H -0.0308 0.5519 -0.0805 0.071 Uiso 1 1 calc R . .
C18 C -0.1350(9) 0.6542(5) -0.0791(5) 0.062(2) Uani 1 1 d . . .
H18 H -0.1911 0.6353 -0.1107 0.074 Uiso 1 1 calc R . .
C19 C -0.1515(7) 0.7310(5) -0.0510(5) 0.0512(19) Uani 1 1 d . . .
H19 H -0.2170 0.7647 -0.0652 0.061 Uiso 1 1 calc R . .
C20 C -0.0717(6) 0.7589(4) -0.0020(4) 0.0367(15) Uani 1 1 d . . .
C21 C -0.2439(6) 0.7168(5) 0.1669(5) 0.0466(17) Uani 1 1 d . . .
H21 H -0.2812 0.7632 0.1355 0.056 Uiso 1 1 calc R . .
C22 C -0.3070(7) 0.6443(5) 0.1997(6) 0.061(2) Uani 1 1 d . . .
H22 H -0.3862 0.6416 0.1908 0.073 Uiso 1 1 calc R . .
C23 C -0.2542(8) 0.5760(5) 0.2454(6) 0.064(2) Uani 1 1 d . . .
C24 C -0.1385(8) 0.5812(5) 0.2523(5) 0.056(2) Uani 1 1 d . . .
H24 H -0.0984 0.5341 0.2802 0.067 Uiso 1 1 calc R . .
C25 C -0.0798(6) 0.6556(4) 0.2186(4) 0.0403(15) Uani 1 1 d . . .
H25 H 0.0003 0.6581 0.2246 0.048 Uiso 1 1 calc R . .
C26 C -0.3231(10) 0.4980(6) 0.2866(8) 0.094(4) Uani 1 1 d . . .
H26A H -0.3516 0.4688 0.2445 0.141 Uiso 1 1 calc R . .
H26B H -0.3880 0.5156 0.3202 0.141 Uiso 1 1 calc R . .
H26C H -0.2739 0.4593 0.3214 0.141 Uiso 1 1 calc R . .
C27 C 0.2127(5) 0.9685(4) 0.3527(4) 0.0349(14) Uani 1 1 d . . .
C28 C 0.3263(6) 0.9965(6) 0.3267(4) 0.0495(19) Uani 1 1 d . . .
H28 H 0.3880 0.9578 0.3372 0.059 Uiso 1 1 calc R . .
C29 C 0.3496(7) 1.0775(6) 0.2868(5) 0.055(2) Uani 1 1 d . . .
H29 H 0.4269 1.0941 0.2715 0.066 Uiso 1 1 calc R . .
C30 C 0.2621(7) 1.1361(5) 0.2682(5) 0.054(2) Uani 1 1 d . . .
H30 H 0.2784 1.1913 0.2381 0.065 Uiso 1 1 calc R . .
C31 C 0.1521(7) 1.1120(4) 0.2945(4) 0.0418(16) Uani 1 1 d . . .
H31 H 0.0923 1.1523 0.2831 0.050 Uiso 1 1 calc R . .
C32 C 0.1233(5) 1.0299(4) 0.3378(4) 0.0329(13) Uani 1 1 d . . .
C33 C 0.0051(5) 1.0190(4) 0.3671(4) 0.0287(13) Uani 1 1 d . . .
H33 H -0.0443 1.0663 0.3538 0.034 Uiso 1 1 calc R . .
C34 C -0.1637(5) 0.9466(4) 0.4377(4) 0.0298(13) Uani 1 1 d . . .
H34 H -0.1695 0.9538 0.4965 0.036 Uiso 1 1 calc R . .
C35 C -0.2411(5) 1.0127(4) 0.3923(4) 0.0375(15) Uani 1 1 d . . .
H35A H -0.2346 1.0095 0.3331 0.045 Uiso 1 1 calc R . .
H35B H -0.2170 1.0703 0.3989 0.045 Uiso 1 1 calc R . .
C36 C -0.3663(6) 0.9969(6) 0.4262(5) 0.0524(19) Uani 1 1 d . . .
H36A H -0.3740 1.0075 0.4834 0.063 Uiso 1 1 calc R . .
H36B H -0.4166 1.0377 0.3934 0.063 Uiso 1 1 calc R . .
C37 C -0.4053(6) 0.9074(6) 0.4243(5) 0.054(2) Uani 1 1 d . . .
H37A H -0.4037 0.8979 0.3667 0.065 Uiso 1 1 calc R . .
H37B H -0.4852 0.8996 0.4481 0.065 Uiso 1 1 calc R . .
C38 C -0.3276(6) 0.8426(5) 0.4727(4) 0.0466(17) Uani 1 1 d . . .
H38A H -0.3531 0.7841 0.4706 0.056 Uiso 1 1 calc R . .
H38B H -0.3310 0.8503 0.5308 0.056 Uiso 1 1 calc R . .
C39 C -0.2048(5) 0.8566(4) 0.4345(4) 0.0350(14) Uani 1 1 d . . .
H39 H -0.2041 0.8495 0.3757 0.042 Uiso 1 1 calc R . .
C40 C -0.1376(6) 0.7536(4) 0.5464(4) 0.0400(15) Uani 1 1 d . . .
H40 H -0.2152 0.7396 0.5635 0.048 Uiso 1 1 calc R . .
C41 C -0.0510(6) 0.7227(4) 0.6012(4) 0.0400(16) Uani 1 1 d . . .
C42 C -0.0787(8) 0.6554(5) 0.6670(4) 0.0493(18) Uani 1 1 d . . .
H42 H -0.1491 0.6259 0.6689 0.059 Uiso 1 1 calc R . .
C43 C -0.0049(9) 0.6324(5) 0.7280(5) 0.062(2) Uani 1 1 d . . .
H43 H -0.0222 0.5852 0.7702 0.075 Uiso 1 1 calc R . .
C44 C 0.0935(9) 0.6778(5) 0.7276(5) 0.059(2) Uani 1 1 d . . .
H44 H 0.1428 0.6631 0.7711 0.071 Uiso 1 1 calc R . .
C45 C 0.1229(7) 0.7448(5) 0.6651(4) 0.0500(18) Uani 1 1 d . . .
H45 H 0.1918 0.7755 0.6662 0.060 Uiso 1 1 calc R . .
C46 C 0.0515(6) 0.7678(4) 0.6001(4) 0.0388(15) Uani 1 1 d . . .
C47 C 0.0636(8) 0.6490(5) 0.4182(5) 0.053(2) Uani 1 1 d . . .
H47 H -0.0081 0.6583 0.3945 0.064 Uiso 1 1 calc R . .
C48 C 0.1079(11) 0.5678(5) 0.4298(6) 0.078(3) Uani 1 1 d . C .
H48 H 0.0675 0.5228 0.4136 0.093 Uiso 1 1 calc R . .
C49 C 0.2115(11) 0.5523(6) 0.4652(5) 0.082(4) Uani 1 1 d . . .
C50 C 0.2652(9) 0.6198(6) 0.4862(5) 0.066(3) Uani 1 1 d . C .
H50 H 0.3364 0.6115 0.5108 0.080 Uiso 1 1 calc R . .
C51 C 0.2180(7) 0.6997(5) 0.4726(5) 0.0510(19) Uani 1 1 d . . .
H51 H 0.2583 0.7455 0.4875 0.061 Uiso 1 1 calc R C .
C52A C 0.294(3) 0.476(2) 0.469(3) 0.078(11) Uani 0.40 1 d PU C 1
H52A H 0.3699 0.4952 0.4463 0.117 Uiso 0.40 1 calc PR C 1
H52B H 0.2647 0.4346 0.4380 0.117 Uiso 0.40 1 calc PR C 1
H52C H 0.2983 0.4485 0.5268 0.117 Uiso 0.40 1 calc PR C 1
C52B C 0.242(2) 0.4557(16) 0.4854(19) 0.074(7) Uani 0.60 1 d PU C 2
H52D H 0.2902 0.4397 0.4397 0.111 Uiso 0.60 1 calc PR C 2
H52E H 0.1719 0.4218 0.4941 0.111 Uiso 0.60 1 calc PR C 2
H52F H 0.2846 0.4452 0.5353 0.111 Uiso 0.60 1 calc PR C 2
N9 N 0.4449(14) 0.3337(9) 0.5954(10) 0.156(6) Uani 1 1 d . . .
C53 C 0.5772(15) 0.2479(8) 0.6949(8) 0.126(6) Uani 1 1 d . . .
H53A H 0.6231 0.2091 0.6661 0.189 Uiso 1 1 calc R . .
H53B H 0.5313 0.2150 0.7409 0.189 Uiso 1 1 calc R . .
H53C H 0.6281 0.2865 0.7156 0.189 Uiso 1 1 calc R . .
C54 C 0.5049(13) 0.2949(8) 0.6412(8) 0.100(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
Os1 0.02466(14) 0.02766(14) 0.02191(14) -0.00177(10) -0.00052(9) -0.00191(10)
Os2 0.02894(14) 0.03048(14) 0.02173(14) -0.00468(10) -0.00101(10) 0.00392(10)
P1A 0.076(4) 0.044(3) 0.066(3) -0.003(2) -0.025(3) -0.007(2)
F1A 0.088(6) 0.060(4) 0.085(6) -0.007(4) -0.010(4) 0.008(4)
F2A 0.154(10) 0.191(10) 0.244(11) -0.036(9) -0.019(9) -0.017(8)
F3A 0.188(9) 0.124(8) 0.116(8) -0.004(6) 0.013(7) 0.018(7)
F4A 0.106(8) 0.173(9) 0.185(10) -0.024(8) -0.023(7) -0.031(7)
F5A 0.169(9) 0.138(9) 0.109(8) -0.002(7) -0.021(7) 0.022(8)
F6A 0.134(8) 0.079(6) 0.131(7) -0.043(5) -0.030(6) 0.026(6)
P1B 0.073(8) 0.068(7) 0.083(8) -0.002(5) -0.030(5) -0.007(5)
F1B 0.21(2) 0.21(2) 0.21(2) -0.040(11) -0.014(10) 0.018(10)
F2B 0.180(15) 0.177(15) 0.183(15) 0.002(10) -0.021(10) -0.037(10)
F3B 0.087(8) 0.091(8) 0.066(8) -0.012(7) -0.034(7) 0.009(7)
F4B 0.090(9) 0.082(8) 0.106(9) 0.010(7) 0.003(8) -0.002(7)
F5B 0.128(11) 0.126(11) 0.097(10) -0.015(8) -0.055(8) -0.019(9)
F6B 0.107(9) 0.093(9) 0.090(9) -0.015(7) 0.000(8) 0.030(8)
O1 0.043(3) 0.036(2) 0.022(2) -0.0033(17) -0.0071(18) -0.0041(19)
O2 0.043(2) 0.038(2) 0.019(2) -0.0046(17) -0.0064(18) 0.0050(19)
O3 0.023(2) 0.040(2) 0.040(2) -0.0033(19) 0.0004(18) -0.0033(18)
O4 0.021(2) 0.047(3) 0.037(2) -0.004(2) 0.0017(18) 0.0058(19)
N1 0.026(2) 0.029(3) 0.020(3) -0.0017(19) 0.0061(19) 0.003(2)
N2 0.033(3) 0.030(3) 0.016(3) -0.0027(19) 0.0016(19) 0.002(2)
N3 0.024(2) 0.027(2) 0.027(3) -0.0007(19) -0.0041(19) -0.0031(19)
N4 0.029(3) 0.032(3) 0.024(3) 0.000(2) -0.001(2) -0.002(2)
N5 0.035(3) 0.029(3) 0.032(3) -0.002(2) -0.001(2) -0.005(2)
N6 0.025(2) 0.030(3) 0.023(2) -0.010(2) 0.0007(19) 0.003(2)
N7 0.034(3) 0.039(3) 0.027(3) -0.011(2) -0.004(2) -0.001(2)
N8 0.059(4) 0.033(3) 0.028(3) -0.007(2) -0.004(3) 0.011(3)
C1 0.028(3) 0.038(3) 0.025(3) -0.002(2) 0.001(2) 0.004(3)
C2 0.026(3) 0.054(4) 0.034(4) -0.005(3) 0.000(3) 0.003(3)
C3 0.036(4) 0.053(4) 0.048(4) -0.006(3) 0.005(3) 0.015(3)
C4 0.050(4) 0.039(4) 0.048(4) -0.010(3) 0.004(3) 0.013(3)
C5 0.041(4) 0.038(3) 0.033(3) -0.007(3) 0.001(3) 0.005(3)
C6 0.031(3) 0.033(3) 0.024(3) -0.003(2) -0.002(2) 0.001(2)
C7 0.035(3) 0.033(3) 0.020(3) -0.002(2) -0.005(2) 0.005(3)
C8 0.024(3) 0.031(3) 0.026(3) -0.002(2) 0.001(2) -0.001(2)
C9 0.025(3) 0.035(3) 0.037(3) -0.003(3) -0.001(3) -0.006(3)
C10 0.028(3) 0.045(4) 0.042(4) -0.008(3) 0.004(3) -0.004(3)
C11 0.026(3) 0.049(4) 0.057(5) -0.002(3) 0.001(3) 0.003(3)
C12 0.030(3) 0.043(4) 0.047(4) -0.007(3) 0.004(3) 0.005(3)
C13 0.027(3) 0.036(3) 0.024(3) -0.004(2) 0.000(2) -0.001(2)
C14 0.039(4) 0.033(3) 0.034(3) -0.008(3) 0.003(3) 0.003(3)
C15 0.055(4) 0.035(3) 0.028(3) -0.006(3) 0.001(3) -0.004(3)
C16 0.068(5) 0.039(4) 0.043(4) -0.018(3) 0.002(4) -0.001(4)
C17 0.092(7) 0.045(4) 0.044(4) -0.020(4) -0.002(4) -0.008(4)
C18 0.091(7) 0.058(5) 0.041(4) -0.017(4) -0.012(4) -0.025(5)
C19 0.064(5) 0.050(4) 0.041(4) -0.006(3) -0.016(4) -0.014(4)
C20 0.050(4) 0.039(4) 0.021(3) -0.005(3) -0.002(3) -0.011(3)
C21 0.041(4) 0.045(4) 0.052(4) -0.001(3) -0.006(3) -0.006(3)
C22 0.043(4) 0.049(5) 0.088(6) -0.003(4) -0.006(4) -0.017(4)
C23 0.064(6) 0.041(4) 0.080(6) 0.000(4) 0.009(5) -0.016(4)
C24 0.066(5) 0.033(4) 0.064(5) 0.006(3) -0.006(4) -0.006(4)
C25 0.044(4) 0.033(3) 0.042(4) -0.002(3) -0.001(3) -0.002(3)
C26 0.092(8) 0.048(5) 0.132(10) 0.012(6) -0.002(7) -0.028(5)
C27 0.032(3) 0.052(4) 0.024(3) -0.014(3) -0.001(2) -0.003(3)
C28 0.030(4) 0.079(6) 0.040(4) -0.014(4) 0.001(3) -0.004(4)
C29 0.036(4) 0.081(6) 0.047(4) -0.016(4) 0.009(3) -0.027(4)
C30 0.061(5) 0.053(5) 0.048(4) -0.011(4) 0.008(4) -0.024(4)
C31 0.055(4) 0.042(4) 0.028(3) -0.008(3) 0.004(3) -0.007(3)
C32 0.036(3) 0.040(3) 0.022(3) -0.005(3) 0.001(2) -0.003(3)
C33 0.031(3) 0.029(3) 0.027(3) -0.009(2) -0.002(2) 0.006(2)
C34 0.023(3) 0.046(4) 0.021(3) -0.010(3) 0.002(2) 0.001(3)
C35 0.031(3) 0.045(4) 0.037(4) -0.011(3) -0.003(3) 0.009(3)
C36 0.030(4) 0.076(5) 0.054(5) -0.019(4) -0.005(3) 0.019(4)
C37 0.023(3) 0.085(6) 0.054(5) -0.014(4) 0.001(3) 0.001(4)
C38 0.029(3) 0.069(5) 0.041(4) -0.009(3) 0.005(3) -0.010(3)
C39 0.024(3) 0.050(4) 0.029(3) -0.003(3) 0.004(2) -0.004(3)
C40 0.048(4) 0.041(4) 0.029(3) -0.004(3) 0.006(3) -0.011(3)
C41 0.059(4) 0.036(3) 0.024(3) -0.004(3) 0.004(3) 0.001(3)
C42 0.074(5) 0.042(4) 0.029(4) -0.004(3) 0.006(3) -0.003(4)
C43 0.104(8) 0.051(5) 0.028(4) 0.003(3) -0.002(4) 0.006(5)
C44 0.086(6) 0.062(5) 0.028(4) -0.004(3) -0.014(4) 0.019(5)
C45 0.064(5) 0.053(4) 0.032(4) -0.004(3) -0.010(3) 0.010(4)
C46 0.058(4) 0.035(3) 0.025(3) -0.009(3) -0.005(3) 0.012(3)
C47 0.083(6) 0.036(4) 0.044(4) -0.014(3) -0.012(4) 0.006(4)
C48 0.135(10) 0.042(5) 0.063(6) -0.019(4) -0.033(6) 0.026(5)
C49 0.147(11) 0.057(6) 0.044(5) -0.015(4) -0.020(6) 0.047(6)
C50 0.089(7) 0.067(6) 0.042(5) -0.008(4) -0.007(4) 0.036(5)
C51 0.055(5) 0.053(4) 0.045(4) -0.007(3) -0.008(3) 0.022(4)
C52A 0.11(3) 0.047(19) 0.08(2) -0.008(15) -0.02(2) 0.040(19)
C52B 0.104(19) 0.042(11) 0.075(14) -0.010(9) -0.007(13) 0.010(11)
N9 0.176(14) 0.135(11) 0.165(13) -0.026(10) -0.081(11) 0.027(10)
C53 0.208(17) 0.087(9) 0.088(9) -0.016(7) -0.051(10) 0.024(10)
C54 0.128(11) 0.078(8) 0.101(9) -0.021(7) -0.047(8) 0.014(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
Os1 N1 1.895(5) . ?
Os1 N3 2.014(5) . ?
Os1 O1 2.028(4) . ?
Os1 N4 2.034(5) . ?
Os1 O3 2.046(4) . ?
Os1 N5 2.090(5) . ?
Os2 N2 1.888(5) . ?
Os2 N7 2.017(5) . ?
Os2 O2 2.018(4) . ?
Os2 N6 2.035(5) . ?
Os2 O4 2.048(4) . ?
Os2 N8 2.098(5) . ?
P1A F4A 1.543(11) . ?
P1A F3A 1.556(11) . ?
P1A F2A 1.567(13) . ?
P1A F6A 1.568(10) . ?
P1A F5A 1.574(11) . ?
P1A F1A 1.578(10) . ?
P1B F4B 1.548(15) . ?
P1B F6B 1.556(15) . ?
P1B F2B 1.565(16) . ?
P1B F5B 1.571(15) . ?
P1B F3B 1.572(15) . ?
P1B F1B 1.600(16) . ?
O1 C20 1.320(8) . ?
O2 C46 1.342(8) . ?
O3 C1 1.321(7) . ?
O4 C27 1.311(8) . ?
N1 N2 1.135(7) . ?
N3 C7 1.282(8) . ?
N3 C8 1.505(7) . ?
N4 C14 1.288(8) . ?
N4 C13 1.481(8) . ?
N5 C25 1.331(8) . ?
N5 C21 1.357(9) . ?
N6 C33 1.278(8) . ?
N6 C34 1.494(7) . ?
N7 C40 1.297(8) . ?
N7 C39 1.490(8) . ?
N8 C47 1.344(9) . ?
N8 C51 1.346(9) . ?
C1 C6 1.418(9) . ?
C1 C2 1.421(8) . ?
C2 C3 1.370(10) . ?
C2 H2 0.9500 . ?
C3 C4 1.377(11) . ?
C3 H3 0.9500 . ?
C4 C5 1.378(9) . ?
C4 H4 0.9500 . ?
C5 C6 1.411(9) . ?
C5 H5 0.9500 . ?
C6 C7 1.440(8) . ?
C7 H7 0.9500 . ?
C8 C9 1.522(8) . ?
C8 C13 1.542(8) . ?
C8 H8 1.0000 . ?
C9 C10 1.535(8) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.512(9) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.535(10) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.528(8) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13 1.0000 . ?
C14 C15 1.436(9) . ?
C14 H14 0.9500 . ?
C15 C16 1.408(9) . ?
C15 C20 1.421(10) . ?
C16 C17 1.371(11) . ?
C16 H16 0.9500 . ?
C17 C18 1.376(13) . ?
C17 H17 0.9500 . ?
C18 C19 1.391(11) . ?
C18 H18 0.9500 . ?
C19 C20 1.403(9) . ?
C19 H19 0.9500 . ?
C21 C22 1.389(10) . ?
C21 H21 0.9500 . ?
C22 C23 1.381(12) . ?
C22 H22 0.9500 . ?
C23 C24 1.371(12) . ?
C23 C26 1.524(11) . ?
C24 C25 1.390(10) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.422(9) . ?
C27 C32 1.429(9) . ?
C28 C29 1.369(11) . ?
C28 H28 0.9500 . ?
C29 C30 1.392(12) . ?
C29 H29 0.9500 . ?
C30 C31 1.367(11) . ?
C30 H30 0.9500 . ?
C31 C32 1.415(9) . ?
C31 H31 0.9500 . ?
C32 C33 1.436(9) . ?
C33 H33 0.9500 . ?
C34 C35 1.516(8) . ?
C34 C39 1.530(9) . ?
C34 H34 1.0000 . ?
C35 C36 1.540(10) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 C37 1.512(12) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 C38 1.528(11) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 C39 1.532(9) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 H39 1.0000 . ?
C40 C41 1.433(10) . ?
C40 H40 0.9500 . ?
C41 C46 1.403(10) . ?
C41 C42 1.417(9) . ?
C42 C43 1.374(12) . ?
C42 H42 0.9500 . ?
C43 C44 1.365(13) . ?
C43 H43 0.9500 . ?
C44 C45 1.385(11) . ?
C44 H44 0.9500 . ?
C45 C46 1.405(10) . ?
C45 H45 0.9500 . ?
C47 C48 1.376(11) . ?
C47 H47 0.9500 . ?
C48 C49 1.383(15) . ?
C48 H48 0.9500 . ?
C49 C50 1.359(15) . ?
C49 C52A 1.54(4) . ?
C49 C52B 1.56(3) . ?
C50 C51 1.373(11) . ?
C50 H50 0.9500 . ?
C51 H51 0.9500 . ?
C52A H52A 0.9800 . ?
C52A H52B 0.9800 . ?
C52A H52C 0.9800 . ?
C52B H52D 0.9800 . ?
C52B H52E 0.9800 . ?
C52B H52F 0.9800 . ?
N9 C54 1.163(15) . ?
C53 C54 1.389(16) . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
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
N1 Os1 N3 87.8(2) . . ?
N1 Os1 O1 175.46(18) . . ?
N3 Os1 O1 96.76(18) . . ?
N1 Os1 N4 95.76(19) . . ?
N3 Os1 N4 80.5(2) . . ?
O1 Os1 N4 85.02(19) . . ?
N1 Os1 O3 92.24(18) . . ?
N3 Os1 O3 93.42(18) . . ?
O1 Os1 O3 87.51(18) . . ?
N4 Os1 O3 169.70(18) . . ?
N1 Os1 N5 88.9(2) . . ?
N3 Os1 N5 176.65(19) . . ?
O1 Os1 N5 86.56(19) . . ?
N4 Os1 N5 99.4(2) . . ?
O3 Os1 N5 87.16(19) . . ?
N2 Os2 N7 96.6(2) . . ?
N2 Os2 O2 176.77(19) . . ?
N7 Os2 O2 85.47(19) . . ?
N2 Os2 N6 85.26(19) . . ?
N7 Os2 N6 80.5(2) . . ?
O2 Os2 N6 97.58(18) . . ?
N2 Os2 O4 90.83(19) . . ?
N7 Os2 O4 170.09(19) . . ?
O2 Os2 O4 87.46(18) . . ?
N6 Os2 O4 93.59(18) . . ?
N2 Os2 N8 92.7(2) . . ?
N7 Os2 N8 97.2(2) . . ?
O2 Os2 N8 84.55(19) . . ?
N6 Os2 N8 176.7(2) . . ?
O4 Os2 N8 89.1(2) . . ?
F4A P1A F3A 89.7(8) . . ?
F4A P1A F2A 179.2(10) . . ?
F3A P1A F2A 89.8(8) . . ?
F4A P1A F6A 93.1(8) . . ?
F3A P1A F6A 86.7(7) . . ?
F2A P1A F6A 87.4(7) . . ?
F4A P1A F5A 89.9(8) . . ?
F3A P1A F5A 178.4(9) . . ?
F2A P1A F5A 90.6(8) . . ?
F6A P1A F5A 91.8(7) . . ?
F4A P1A F1A 91.8(7) . . ?
F3A P1A F1A 92.0(7) . . ?
F2A P1A F1A 87.7(8) . . ?
F6A P1A F1A 174.9(9) . . ?
F5A P1A F1A 89.5(6) . . ?
F4B P1B F6B 88.9(10) . . ?
F4B P1B F2B 179.3(14) . . ?
F6B P1B F2B 91.1(11) . . ?
F4B P1B F5B 92.2(10) . . ?
F6B P1B F5B 93.9(11) . . ?
F2B P1B F5B 88.5(10) . . ?
F4B P1B F3B 91.1(10) . . ?
F6B P1B F3B 91.9(10) . . ?
F2B P1B F3B 88.1(10) . . ?
F5B P1B F3B 173.4(13) . . ?
F4B P1B F1B 90.5(11) . . ?
F6B P1B F1B 179.1(14) . . ?
F2B P1B F1B 89.4(11) . . ?
F5B P1B F1B 86.9(10) . . ?
F3B P1B F1B 87.4(10) . . ?
C20 O1 Os1 117.6(4) . . ?
C46 O2 Os2 120.1(4) . . ?
C1 O3 Os1 122.6(4) . . ?
C27 O4 Os2 122.1(4) . . ?
N2 N1 Os1 176.8(5) . . ?
N1 N2 Os2 176.6(4) . . ?
C7 N3 C8 120.7(5) . . ?
C7 N3 Os1 124.5(4) . . ?
C8 N3 Os1 114.3(3) . . ?
C14 N4 C13 122.2(5) . . ?
C14 N4 Os1 124.9(4) . . ?
C13 N4 Os1 110.4(4) . . ?
C25 N5 C21 117.2(6) . . ?
C25 N5 Os1 122.4(4) . . ?
C21 N5 Os1 120.2(4) . . ?
C33 N6 C34 121.7(5) . . ?
C33 N6 Os2 123.4(4) . . ?
C34 N6 Os2 113.9(4) . . ?
C40 N7 C39 121.0(6) . . ?
C40 N7 Os2 125.3(5) . . ?
C39 N7 Os2 110.2(4) . . ?
C47 N8 C51 116.4(6) . . ?
C47 N8 Os2 121.7(5) . . ?
C51 N8 Os2 121.8(5) . . ?
O3 C1 C6 126.0(5) . . ?
O3 C1 C2 116.0(6) . . ?
C6 C1 C2 118.0(6) . . ?
C3 C2 C1 120.6(7) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C2 C3 C4 122.0(6) . . ?
C2 C3 H3 119.0 . . ?
C4 C3 H3 119.0 . . ?
C3 C4 C5 118.5(7) . . ?
C3 C4 H4 120.8 . . ?
C5 C4 H4 120.8 . . ?
C4 C5 C6 122.2(7) . . ?
C4 C5 H5 118.9 . . ?
C6 C5 H5 118.9 . . ?
C5 C6 C1 118.5(6) . . ?
C5 C6 C7 115.2(6) . . ?
C1 C6 C7 126.2(6) . . ?
N3 C7 C6 125.6(6) . . ?
N3 C7 H7 117.2 . . ?
C6 C7 H7 117.2 . . ?
N3 C8 C9 116.1(5) . . ?
N3 C8 C13 107.5(4) . . ?
C9 C8 C13 111.2(5) . . ?
N3 C8 H8 107.2 . . ?
C9 C8 H8 107.2 . . ?
C13 C8 H8 107.2 . . ?
C8 C9 C10 110.3(5) . . ?
C8 C9 H9A 109.6 . . ?
C10 C9 H9A 109.6 . . ?
C8 C9 H9B 109.6 . . ?
C10 C9 H9B 109.6 . . ?
H9A C9 H9B 108.1 . . ?
C11 C10 C9 112.1(5) . . ?
C11 C10 H10A 109.2 . . ?
C9 C10 H10A 109.2 . . ?
C11 C10 H10B 109.2 . . ?
C9 C10 H10B 109.2 . . ?
H10A C10 H10B 107.9 . . ?
C10 C11 C12 111.0(6) . . ?
C10 C11 H11A 109.4 . . ?
C12 C11 H11A 109.4 . . ?
C10 C11 H11B 109.4 . . ?
C12 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
C13 C12 C11 108.4(5) . . ?
C13 C12 H12A 110.0 . . ?
C11 C12 H12A 110.0 . . ?
C13 C12 H12B 110.0 . . ?
C11 C12 H12B 110.0 . . ?
H12A C12 H12B 108.4 . . ?
N4 C13 C12 117.1(5) . . ?
N4 C13 C8 104.0(4) . . ?
C12 C13 C8 110.1(5) . . ?
N4 C13 H13 108.4 . . ?
C12 C13 H13 108.4 . . ?
C8 C13 H13 108.4 . . ?
N4 C14 C15 122.6(6) . . ?
N4 C14 H14 118.7 . . ?
C15 C14 H14 118.7 . . ?
C16 C15 C20 119.5(7) . . ?
C16 C15 C14 119.4(7) . . ?
C20 C15 C14 120.7(6) . . ?
C17 C16 C15 121.2(8) . . ?
C17 C16 H16 119.4 . . ?
C15 C16 H16 119.4 . . ?
C16 C17 C18 119.2(7) . . ?
C16 C17 H17 120.4 . . ?
C18 C17 H17 120.4 . . ?
C17 C18 C19 121.7(8) . . ?
C17 C18 H18 119.2 . . ?
C19 C18 H18 119.2 . . ?
C18 C19 C20 120.2(8) . . ?
C18 C19 H19 119.9 . . ?
C20 C19 H19 119.9 . . ?
O1 C20 C19 118.1(7) . . ?
O1 C20 C15 123.7(6) . . ?
C19 C20 C15 118.1(6) . . ?
N5 C21 C22 122.2(7) . . ?
N5 C21 H21 118.9 . . ?
C22 C21 H21 118.9 . . ?
C23 C22 C21 119.7(8) . . ?
C23 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
C24 C23 C22 117.7(7) . . ?
C24 C23 C26 121.5(8) . . ?
C22 C23 C26 120.8(9) . . ?
C23 C24 C25 119.9(7) . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
N5 C25 C24 122.9(7) . . ?
N5 C25 H25 118.5 . . ?
C24 C25 H25 118.5 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O4 C27 C28 117.0(6) . . ?
O4 C27 C32 126.1(6) . . ?
C28 C27 C32 116.9(6) . . ?
C29 C28 C27 122.0(7) . . ?
C29 C28 H28 119.0 . . ?
C27 C28 H28 119.0 . . ?
C28 C29 C30 121.2(7) . . ?
C28 C29 H29 119.4 . . ?
C30 C29 H29 119.4 . . ?
C31 C30 C29 118.3(7) . . ?
C31 C30 H30 120.9 . . ?
C29 C30 H30 120.9 . . ?
C30 C31 C32 122.9(7) . . ?
C30 C31 H31 118.5 . . ?
C32 C31 H31 118.5 . . ?
C31 C32 C27 118.6(6) . . ?
C31 C32 C33 114.8(6) . . ?
C27 C32 C33 126.4(6) . . ?
N6 C33 C32 125.7(5) . . ?
N6 C33 H33 117.1 . . ?
C32 C33 H33 117.1 . . ?
N6 C34 C35 116.4(5) . . ?
N6 C34 C39 107.4(5) . . ?
C35 C34 C39 110.9(5) . . ?
N6 C34 H34 107.3 . . ?
C35 C34 H34 107.3 . . ?
C39 C34 H34 107.3 . . ?
C34 C35 C36 110.0(6) . . ?
C34 C35 H35A 109.7 . . ?
C36 C35 H35A 109.7 . . ?
C34 C35 H35B 109.7 . . ?
C36 C35 H35B 109.7 . . ?
H35A C35 H35B 108.2 . . ?
C37 C36 C35 112.3(6) . . ?
C37 C36 H36A 109.1 . . ?
C35 C36 H36A 109.1 . . ?
C37 C36 H36B 109.1 . . ?
C35 C36 H36B 109.1 . . ?
H36A C36 H36B 107.9 . . ?
C36 C37 C38 110.5(6) . . ?
C36 C37 H37A 109.5 . . ?
C38 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
C38 C37 H37B 109.5 . . ?
H37A C37 H37B 108.1 . . ?
C37 C38 C39 108.2(6) . . ?
C37 C38 H38A 110.1 . . ?
C39 C38 H38A 110.1 . . ?
C37 C38 H38B 110.1 . . ?
C39 C38 H38B 110.1 . . ?
H38A C38 H38B 108.4 . . ?
N7 C39 C34 104.6(5) . . ?
N7 C39 C38 115.9(5) . . ?
C34 C39 C38 110.8(6) . . ?
N7 C39 H39 108.4 . . ?
C34 C39 H39 108.4 . . ?
C38 C39 H39 108.4 . . ?
N7 C40 C41 123.6(6) . . ?
N7 C40 H40 118.2 . . ?
C41 C40 H40 118.2 . . ?
C46 C41 C42 119.2(7) . . ?
C46 C41 C40 120.8(6) . . ?
C42 C41 C40 118.8(7) . . ?
C43 C42 C41 120.9(8) . . ?
C43 C42 H42 119.6 . . ?
C41 C42 H42 119.6 . . ?
C44 C43 C42 119.5(8) . . ?
C44 C43 H43 120.2 . . ?
C42 C43 H43 120.2 . . ?
C43 C44 C45 121.4(8) . . ?
C43 C44 H44 119.3 . . ?
C45 C44 H44 119.3 . . ?
C44 C45 C46 120.5(8) . . ?
C44 C45 H45 119.8 . . ?
C46 C45 H45 119.8 . . ?
O2 C46 C41 123.2(6) . . ?
O2 C46 C45 118.3(7) . . ?
C41 C46 C45 118.4(7) . . ?
N8 C47 C48 123.3(9) . . ?
N8 C47 H47 118.4 . . ?
C48 C47 H47 118.4 . . ?
C47 C48 C49 119.6(9) . . ?
C47 C48 H48 120.2 . . ?
C49 C48 H48 120.2 . . ?
C50 C49 C48 117.2(8) . . ?
C50 C49 C52A 110.1(19) . . ?
C48 C49 C52A 131.3(19) . . ?
C50 C49 C52B 128.7(14) . . ?
C48 C49 C52B 113.7(14) . . ?
C52A C49 C52B 25.9(16) . . ?
C49 C50 C51 121.0(9) . . ?
C49 C50 H50 119.5 . . ?
C51 C50 H50 119.5 . . ?
N8 C51 C50 122.5(9) . . ?
N8 C51 H51 118.7 . . ?
C50 C51 H51 118.7 . . ?
C49 C52A H52A 109.5 . . ?
C49 C52A H52B 109.5 . . ?
C49 C52A H52C 109.5 . . ?
C49 C52B H52D 109.5 . . ?
C49 C52B H52E 109.5 . . ?
H52D C52B H52E 109.5 . . ?
C49 C52B H52F 109.5 . . ?
H52D C52B H52F 109.5 . . ?
H52E C52B H52F 109.5 . . ?
C54 C53 H53A 109.5 . . ?
C54 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C54 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
N9 C54 C53 179.1(17) . . ?
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full 67.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max 2.832
_refine_diff_density_min -0.909
_refine_diff_density_rms 0.123
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.500 1.000 469 109 ' '
2 0.217 0.298 0.643 7 1 ' '
3 0.783 0.702 0.357 7 1 ' '
_platon_squeeze_details
;
;
#==============================================================================
data_14
_database_code_depnum_ccdc_archive 'CCDC 777081'
#TrackingRef '- ALL.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety
'C48 H50 N8 O4 Os2 S2, C4 H10 O, F6 P, 0.13(H4 O2)'
_chemical_formula_sum 'C52 H61 F6 N8 O5.50 Os2 P S2'
_chemical_formula_weight 1475.58
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -1.2165 7.6030 '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 12.9550(10)
_cell_length_b 15.0689(12)
_cell_length_c 16.7304(13)
_cell_angle_alpha 90.1530(10)
_cell_angle_beta 112.6130(10)
_cell_angle_gamma 103.882(2)
_cell_volume 2910.5(4)
_cell_formula_units_Z 2
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 5428
_cell_measurement_theta_min 2.42
_cell_measurement_theta_max 28.16
_exptl_crystal_description block
_exptl_crystal_colour dark-red
_exptl_crystal_size_max 0.26
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.14
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.684
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1452
_exptl_absorpt_coefficient_mu 4.532
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.5606
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_process_details ?
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 293(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 'Smart CCD'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 14387
_diffrn_reflns_av_R_equivalents 0.0219
_diffrn_reflns_av_sigmaI/netI 0.0378
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_theta_min 1.94
_diffrn_reflns_theta_max 25.00
_reflns_number_total 10014
_reflns_number_gt 8313
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'SMART (Bruker, 1998)'
_computing_cell_refinement 'SAINT (Bruker, 1999)'
_computing_data_reduction SAINT
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_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.
The Et~2~O solvent was refined using the following distance restraints:
C---C = 1.50 (2) \%A, C---O = 1.45 (2) \%A and non-bonded distances
C49...O5 = C50...C51 = C52...O5 = 2.50 (2) \%A,
and with SIMU = 0.02 restraint. The H~2~O solvent was refined with
ISOR = 0.01 restraint. The hydroxy H atoms were located in a
difference fourier map and refined with AFIX 3 restraint.
;
_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^)+(0.0620P)^2^+7.7583P] 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 10014
_refine_ls_number_parameters 690
_refine_ls_number_restraints 39
_refine_ls_R_factor_all 0.0472
_refine_ls_R_factor_gt 0.0376
_refine_ls_wR_factor_ref 0.1134
_refine_ls_wR_factor_gt 0.1050
_refine_ls_goodness_of_fit_ref 1.043
_refine_ls_restrained_S_all 1.078
_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
C1 C 1.0805(7) 0.7745(5) -0.0336(5) 0.0507(17) Uani 1 1 d . . .
C2 C 1.0513(8) 0.7380(6) -0.1204(5) 0.067(2) Uani 1 1 d . . .
H2A H 0.9781 0.7336 -0.1633 0.080 Uiso 1 1 calc R . .
C3 C 1.1324(10) 0.7093(6) -0.1399(6) 0.078(3) Uani 1 1 d . . .
H3A H 1.1132 0.6877 -0.1973 0.094 Uiso 1 1 calc R . .
C4 C 1.2395(9) 0.7107(6) -0.0798(6) 0.073(2) Uani 1 1 d . . .
H4A H 1.2914 0.6888 -0.0951 0.088 Uiso 1 1 calc R . .
C5 C 1.2683(8) 0.7453(6) 0.0038(6) 0.064(2) Uani 1 1 d . . .
H5A H 1.3420 0.7483 0.0454 0.077 Uiso 1 1 calc R . .
C6 C 1.1896(6) 0.7768(5) 0.0291(5) 0.0503(16) Uani 1 1 d . . .
C7 C 1.2362(6) 0.8319(5) 0.1120(5) 0.0511(17) Uani 1 1 d . . .
H7A H 1.3162 0.8530 0.1411 0.061 Uiso 1 1 calc R . .
C8 C 1.2132(6) 0.9385(5) 0.2083(4) 0.0445(15) Uani 1 1 d . . .
H8A H 1.1923 0.9241 0.2580 0.053 Uiso 1 1 calc R . .
C9 C 1.3417(6) 0.9862(6) 0.2433(5) 0.0570(19) Uani 1 1 d . . .
H9A H 1.3860 0.9447 0.2749 0.068 Uiso 1 1 calc R . .
H9B H 1.3643 1.0034 0.1954 0.068 Uiso 1 1 calc R . .
C10 C 1.3670(7) 1.0709(6) 0.3031(5) 0.068(2) Uani 1 1 d . . .
H10A H 1.4488 1.1022 0.3242 0.082 Uiso 1 1 calc R . .
H10B H 1.3495 1.0529 0.3530 0.082 Uiso 1 1 calc R . .
C11 C 1.2950(8) 1.1376(6) 0.2561(6) 0.076(3) Uani 1 1 d . . .
H11A H 1.3086 1.1886 0.2975 0.091 Uiso 1 1 calc R . .
H11B H 1.3204 1.1622 0.2112 0.091 Uiso 1 1 calc R . .
C12 C 1.1652(7) 1.0902(5) 0.2146(5) 0.061(2) Uani 1 1 d . . .
H12A H 1.1240 1.1319 0.1800 0.074 Uiso 1 1 calc R . .
H12B H 1.1368 1.0745 0.2599 0.074 Uiso 1 1 calc R . .
C13 C 1.1422(6) 1.0027(5) 0.1565(4) 0.0450(15) Uani 1 1 d . . .
H13A H 1.1687 1.0212 0.1101 0.054 Uiso 1 1 calc R . .
C14 C 0.9351(6) 0.9880(5) 0.0931(4) 0.0460(16) Uani 1 1 d . . .
H14A H 0.9552 1.0511 0.1084 0.055 Uiso 1 1 calc R . .
C15 C 0.8128(6) 0.9425(5) 0.0476(4) 0.0483(16) Uani 1 1 d . . .
C16 C 0.7393(7) 1.0018(6) 0.0293(5) 0.061(2) Uani 1 1 d . . .
H16A H 0.7709 1.0635 0.0510 0.073 Uiso 1 1 calc R . .
C17 C 0.6229(8) 0.9712(8) -0.0193(6) 0.069(2) Uani 1 1 d . . .
H17A H 0.5765 1.0120 -0.0305 0.083 Uiso 1 1 calc R . .
C18 C 0.5745(8) 0.8803(9) -0.0515(6) 0.081(3) Uani 1 1 d . . .
H18A H 0.4956 0.8597 -0.0856 0.097 Uiso 1 1 calc R . .
C19 C 0.6440(7) 0.8187(7) -0.0329(5) 0.069(2) Uani 1 1 d . . .
H19A H 0.6102 0.7572 -0.0548 0.083 Uiso 1 1 calc R . .
C20 C 0.7642(6) 0.8478(6) 0.0182(4) 0.0511(17) Uani 1 1 d . . .
C21 C 0.8825(7) 0.6163(6) 0.0185(6) 0.064(2) Uani 1 1 d . . .
H21A H 0.8344 0.6418 -0.0269 0.077 Uiso 1 1 calc R . .
C22 C 0.9801(9) 0.5199(6) 0.1165(7) 0.082(3) Uani 1 1 d . . .
H22A H 1.0079 0.4735 0.1473 0.099 Uiso 1 1 calc R . .
C23 C 1.0266(7) 0.6106(5) 0.1434(5) 0.0589(19) Uani 1 1 d . . .
C24 C 1.1303(8) 0.6503(6) 0.2243(6) 0.070(2) Uani 1 1 d . . .
H24A H 1.1582 0.6015 0.2550 0.105 Uiso 1 1 calc R . .
H24B H 1.1100 0.6862 0.2606 0.105 Uiso 1 1 calc R . .
H24C H 1.1898 0.6887 0.2096 0.105 Uiso 1 1 calc R . .
C25 C 0.8888(6) 0.7261(5) 0.5210(4) 0.0475(16) Uani 1 1 d . . .
C26 C 0.9186(8) 0.7008(6) 0.6055(5) 0.064(2) Uani 1 1 d . . .
H26A H 0.9933 0.7262 0.6465 0.076 Uiso 1 1 calc R . .
C27 C 0.8428(9) 0.6406(6) 0.6303(6) 0.074(2) Uani 1 1 d . . .
H27A H 0.8660 0.6262 0.6875 0.089 Uiso 1 1 calc R . .
C28 C 0.7294(10) 0.6000(7) 0.5697(7) 0.079(3) Uani 1 1 d . . .
H28A H 0.6780 0.5572 0.5857 0.095 Uiso 1 1 calc R . .
C29 C 0.6966(8) 0.6246(6) 0.4870(6) 0.066(2) Uani 1 1 d . . .
H29A H 0.6207 0.6000 0.4475 0.079 Uiso 1 1 calc R . .
C30 C 0.7741(6) 0.6865(5) 0.4593(5) 0.0512(17) Uani 1 1 d . . .
C31 C 0.7276(6) 0.7246(5) 0.3782(4) 0.0493(16) Uani 1 1 d . . .
H31A H 0.6477 0.7152 0.3510 0.059 Uiso 1 1 calc R . .
C32 C 0.7494(6) 0.8392(5) 0.2817(4) 0.0464(16) Uani 1 1 d . . .
H32A H 0.7704 0.8331 0.2319 0.056 Uiso 1 1 calc R . .
C33 C 0.6214(6) 0.8354(6) 0.2463(5) 0.058(2) Uani 1 1 d . . .
H33A H 0.5984 0.8434 0.2941 0.070 Uiso 1 1 calc R . .
H33B H 0.5760 0.7761 0.2137 0.070 Uiso 1 1 calc R . .
C34 C 0.5997(7) 0.9112(7) 0.1876(6) 0.074(3) Uani 1 1 d . . .
H34A H 0.5182 0.9098 0.1654 0.088 Uiso 1 1 calc R . .
H34B H 0.6188 0.9007 0.1383 0.088 Uiso 1 1 calc R . .
C35 C 0.6714(7) 1.0048(7) 0.2359(6) 0.072(3) Uani 1 1 d . . .
H35A H 0.6451 1.0182 0.2805 0.086 Uiso 1 1 calc R . .
H35B H 0.6590 1.0510 0.1955 0.086 Uiso 1 1 calc R . .
C36 C 0.8004(7) 1.0112(6) 0.2784(6) 0.063(2) Uani 1 1 d . . .
H36A H 0.8304 1.0088 0.2337 0.076 Uiso 1 1 calc R . .
H36B H 0.8410 1.0694 0.3145 0.076 Uiso 1 1 calc R . .
C37 C 0.8215(6) 0.9329(5) 0.3336(4) 0.0485(17) Uani 1 1 d . . .
H37A H 0.7954 0.9403 0.3804 0.058 Uiso 1 1 calc R . .
C38 C 1.0288(6) 1.0011(5) 0.4003(4) 0.0475(16) Uani 1 1 d . . .
H38A H 1.0091 1.0566 0.3897 0.057 Uiso 1 1 calc R . .
C39 C 1.1507(6) 1.0056(5) 0.4424(4) 0.0461(15) Uani 1 1 d . . .
C40 C 1.2280(7) 1.0941(5) 0.4642(5) 0.0548(18) Uani 1 1 d . . .
H40A H 1.1977 1.1442 0.4468 0.066 Uiso 1 1 calc R . .
C41 C 1.3441(7) 1.1101(6) 0.5091(5) 0.060(2) Uani 1 1 d . . .
H41A H 1.3920 1.1696 0.5225 0.072 Uiso 1 1 calc R . .
C42 C 1.3896(7) 1.0349(6) 0.5345(5) 0.062(2) Uani 1 1 d . . .
H42A H 1.4689 1.0449 0.5660 0.074 Uiso 1 1 calc R . .
C43 C 1.3213(6) 0.9476(6) 0.5146(5) 0.0582(19) Uani 1 1 d . . .
H43A H 1.3551 0.8994 0.5332 0.070 Uiso 1 1 calc R . .
C44 C 1.1989(6) 0.9271(5) 0.4658(4) 0.0452(15) Uani 1 1 d . . .
C45 C 1.0811(7) 0.6506(5) 0.4593(5) 0.0549(18) Uani 1 1 d . . .
H45A H 1.1298 0.6954 0.5052 0.066 Uiso 1 1 calc R . .
C46 C 0.9790(8) 0.5158(6) 0.3586(6) 0.069(2) Uani 1 1 d . . .
H46A H 0.9498 0.4583 0.3266 0.082 Uiso 1 1 calc R . .
C47 C 0.9304(7) 0.5864(5) 0.3364(5) 0.0551(18) Uani 1 1 d . . .
C48 C 0.8221(8) 0.5833(6) 0.2563(6) 0.070(2) Uani 1 1 d . . .
H48A H 0.7930 0.5230 0.2250 0.084 Uiso 1 1 calc R . .
H48B H 0.8401 0.6279 0.2195 0.084 Uiso 1 1 calc R . .
H48C H 0.7644 0.5969 0.2735 0.084 Uiso 1 1 calc R . .
C49 C 0.4042(16) 0.6848(14) 0.4922(13) 0.239(11) Uani 1 1 d DU . .
H49A H 0.3479 0.6975 0.4394 0.287 Uiso 1 1 calc R . .
H49B H 0.3995 0.6203 0.4899 0.287 Uiso 1 1 calc R . .
H49C H 0.4804 0.7188 0.4988 0.287 Uiso 1 1 calc R . .
C50 C 0.3803(14) 0.7134(17) 0.5695(10) 0.320(13) Uani 1 1 d DU . .
H50A H 0.4312 0.7748 0.5902 0.383 Uiso 1 1 calc R . .
H50B H 0.3027 0.7218 0.5430 0.383 Uiso 1 1 calc RD . .
C51 C 0.3409(7) 0.6963(6) 0.7064(5) 0.067(2) Uani 1 1 d DU . .
H51A H 0.2577 0.6870 0.6776 0.081 Uiso 1 1 calc R . .
H51B H 0.3744 0.7609 0.7280 0.081 Uiso 1 1 calc R . .
C52 C 0.365(2) 0.6414(16) 0.7826(12) 0.244(10) Uiso 1 1 d DU . .
H52A H 0.3837 0.5870 0.7687 0.293 Uiso 1 1 calc R . .
H52B H 0.2978 0.6243 0.7962 0.293 Uiso 1 1 calc RD . .
H52C H 0.4292 0.6776 0.8319 0.293 Uiso 1 1 calc R . .
F1 F 0.3757(15) 0.4519(15) 0.1519(12) 0.315(10) Uani 1 1 d . . .
F2 F 0.370(2) 0.5886(18) 0.1569(16) 0.441(18) Uani 1 1 d . . .
F3 F 0.2620(10) 0.4797(11) 0.2097(9) 0.230(6) Uani 1 1 d . . .
F4 F 0.4127(14) 0.5994(19) 0.2895(15) 0.374(15) Uani 1 1 d . . .
F5 F 0.5230(10) 0.5473(12) 0.2392(10) 0.250(7) Uani 1 1 d . . .
F6 F 0.419(2) 0.455(2) 0.2942(16) 0.384(15) Uani 1 1 d . . .
N1 N 1.1701(5) 0.8536(4) 0.1479(3) 0.0409(12) Uani 1 1 d . . .
N2 N 1.0184(5) 0.9481(4) 0.1139(3) 0.0425(12) Uani 1 1 d . . .
N3 N 0.9682(5) 0.6666(4) 0.0855(4) 0.0495(14) Uani 1 1 d . . .
N4 N 0.9830(4) 0.8065(3) 0.2083(4) 0.0373(11) Uani 1 1 d . . .
N5 N 0.9738(4) 0.8034(3) 0.2748(4) 0.0373(11) Uani 1 1 d . . .
N6 N 0.7909(5) 0.7711(4) 0.3411(3) 0.0424(12) Uani 1 1 d . . .
N7 N 0.9453(5) 0.9278(4) 0.3762(3) 0.0414(12) Uani 1 1 d . . .
N8 N 0.9904(5) 0.6649(4) 0.3935(4) 0.0460(13) Uani 1 1 d . . .
O1 O 1.0019(4) 0.8076(3) -0.0185(3) 0.0485(11) Uani 1 1 d . . .
O2 O 0.8201(4) 0.7830(4) 0.0338(3) 0.0543(12) Uani 1 1 d . . .
O3 O 0.9656(4) 0.7912(3) 0.5042(3) 0.0462(11) Uani 1 1 d . . .
O4 O 1.1410(4) 0.8422(3) 0.4470(3) 0.0465(11) Uani 1 1 d . . .
O5 O 0.3832(17) 0.6762(14) 0.6427(10) 0.310(9) Uani 1 1 d DU . .
Os1 Os 0.99474(2) 0.810323(17) 0.099566(15) 0.03881(9) Uani 1 1 d . . .
Os2 Os 0.96603(2) 0.799027(17) 0.384554(15) 0.03880(9) Uani 1 1 d . . .
P1 P 0.3958(5) 0.5173(5) 0.2234(3) 0.160(2) Uani 1 1 d . . .
S1 S 0.8647(3) 0.50136(17) 0.0195(2) 0.0943(8) Uani 1 1 d . . .
S2 S 1.1007(2) 0.54467(16) 0.45267(17) 0.0739(6) Uani 1 1 d . . .
O6 O 0.485(5) 0.551(4) -0.016(4) 0.21(2) Uani 0.25 1 d PU . .
H6A H 0.4382 0.5734 -0.0605 0.257 Uiso 0.25 1 d PR . .
H6B H 0.4673 0.4902 -0.0270 0.257 Uiso 0.25 1 d PR . .
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
C1 0.073(5) 0.046(4) 0.044(4) 0.009(3) 0.034(4) 0.016(3)
C2 0.100(6) 0.062(5) 0.048(4) 0.008(4) 0.035(4) 0.029(5)
C3 0.128(9) 0.067(6) 0.065(6) 0.000(4) 0.062(6) 0.031(6)
C4 0.096(7) 0.069(6) 0.081(6) 0.003(5) 0.060(6) 0.025(5)
C5 0.072(5) 0.065(5) 0.072(5) 0.007(4) 0.043(4) 0.022(4)
C6 0.061(4) 0.050(4) 0.049(4) 0.009(3) 0.030(4) 0.017(3)
C7 0.049(4) 0.066(5) 0.047(4) 0.009(3) 0.025(3) 0.020(3)
C8 0.048(4) 0.053(4) 0.035(3) 0.004(3) 0.021(3) 0.011(3)
C9 0.050(4) 0.077(5) 0.043(4) 0.000(4) 0.018(3) 0.016(4)
C10 0.055(5) 0.083(6) 0.053(5) -0.007(4) 0.015(4) 0.005(4)
C11 0.078(6) 0.065(5) 0.063(5) -0.013(4) 0.020(5) -0.005(4)
C12 0.074(5) 0.058(5) 0.056(5) 0.003(4) 0.026(4) 0.022(4)
C13 0.050(4) 0.049(4) 0.035(3) 0.008(3) 0.017(3) 0.009(3)
C14 0.066(4) 0.048(4) 0.037(3) 0.019(3) 0.031(3) 0.022(3)
C15 0.051(4) 0.061(5) 0.042(4) 0.022(3) 0.023(3) 0.021(3)
C16 0.069(5) 0.080(6) 0.064(5) 0.038(4) 0.045(4) 0.041(4)
C17 0.065(5) 0.104(8) 0.063(5) 0.045(5) 0.035(4) 0.048(5)
C18 0.049(5) 0.144(10) 0.063(5) 0.041(6) 0.025(4) 0.043(6)
C19 0.052(4) 0.094(7) 0.058(5) 0.008(4) 0.019(4) 0.016(4)
C20 0.045(4) 0.078(5) 0.036(4) 0.015(3) 0.016(3) 0.026(4)
C21 0.066(5) 0.058(5) 0.064(5) -0.005(4) 0.027(4) 0.009(4)
C22 0.113(8) 0.053(5) 0.095(7) 0.013(5) 0.054(6) 0.027(5)
C23 0.080(5) 0.059(5) 0.060(5) 0.016(4) 0.044(4) 0.030(4)
C24 0.076(6) 0.075(6) 0.071(6) 0.032(5) 0.030(5) 0.038(5)
C25 0.064(4) 0.052(4) 0.045(4) 0.010(3) 0.031(3) 0.035(4)
C26 0.087(6) 0.070(5) 0.045(4) 0.016(4) 0.027(4) 0.038(5)
C27 0.106(7) 0.075(6) 0.063(5) 0.031(5) 0.044(5) 0.044(5)
C28 0.111(8) 0.081(6) 0.081(6) 0.037(5) 0.066(6) 0.043(6)
C29 0.073(5) 0.070(5) 0.073(6) 0.027(4) 0.044(5) 0.028(4)
C30 0.063(4) 0.057(4) 0.052(4) 0.014(3) 0.033(4) 0.030(4)
C31 0.047(4) 0.066(5) 0.045(4) 0.011(3) 0.025(3) 0.019(3)
C32 0.044(4) 0.068(5) 0.036(3) 0.018(3) 0.020(3) 0.024(3)
C33 0.048(4) 0.091(6) 0.048(4) 0.023(4) 0.023(3) 0.031(4)
C34 0.055(5) 0.117(8) 0.058(5) 0.041(5) 0.021(4) 0.040(5)
C35 0.064(5) 0.098(7) 0.073(6) 0.044(5) 0.032(4) 0.048(5)
C36 0.067(5) 0.069(5) 0.069(5) 0.030(4) 0.032(4) 0.037(4)
C37 0.051(4) 0.069(5) 0.041(4) 0.017(3) 0.024(3) 0.032(4)
C38 0.064(4) 0.053(4) 0.040(4) 0.011(3) 0.027(3) 0.032(4)
C39 0.056(4) 0.048(4) 0.040(4) 0.003(3) 0.023(3) 0.019(3)
C40 0.067(5) 0.055(4) 0.049(4) -0.001(3) 0.029(4) 0.019(4)
C41 0.066(5) 0.060(5) 0.056(5) -0.009(4) 0.033(4) 0.008(4)
C42 0.045(4) 0.082(6) 0.051(4) -0.006(4) 0.016(3) 0.008(4)
C43 0.053(4) 0.071(5) 0.049(4) 0.004(4) 0.014(3) 0.023(4)
C44 0.047(4) 0.057(4) 0.034(3) 0.004(3) 0.017(3) 0.017(3)
C45 0.063(5) 0.057(5) 0.055(4) 0.013(3) 0.026(4) 0.030(4)
C46 0.083(6) 0.055(5) 0.077(6) 0.006(4) 0.036(5) 0.025(4)
C47 0.064(5) 0.056(5) 0.052(4) 0.004(3) 0.031(4) 0.017(4)
C48 0.075(6) 0.062(5) 0.068(5) -0.005(4) 0.024(4) 0.015(4)
C49 0.136(13) 0.182(17) 0.40(3) -0.130(18) 0.159(17) -0.047(11)
C50 0.258(17) 0.230(17) 0.238(19) 0.114(15) -0.108(16) -0.006(15)
C51 0.069(5) 0.073(5) 0.031(4) 0.000(3) 0.012(3) -0.020(4)
F1 0.31(2) 0.34(2) 0.249(17) -0.155(17) 0.114(14) -0.008(16)
F2 0.51(4) 0.37(3) 0.30(3) 0.17(2) -0.01(2) 0.14(3)
F3 0.140(9) 0.311(17) 0.249(15) 0.023(12) 0.087(9) 0.060(10)
F4 0.215(16) 0.55(4) 0.31(2) -0.19(2) 0.023(14) 0.16(2)
F5 0.137(9) 0.37(2) 0.241(14) -0.010(14) 0.070(9) 0.067(11)
F6 0.38(3) 0.61(4) 0.33(3) 0.30(3) 0.24(2) 0.27(3)
N1 0.043(3) 0.048(3) 0.038(3) 0.011(2) 0.021(2) 0.015(2)
N2 0.055(3) 0.045(3) 0.036(3) 0.012(2) 0.023(2) 0.018(3)
N3 0.063(4) 0.046(3) 0.051(3) 0.010(3) 0.030(3) 0.021(3)
N4 0.036(3) 0.035(3) 0.044(3) 0.008(2) 0.018(2) 0.011(2)
N5 0.039(3) 0.036(3) 0.044(3) 0.006(2) 0.020(2) 0.016(2)
N6 0.042(3) 0.056(3) 0.033(3) 0.007(2) 0.017(2) 0.017(3)
N7 0.050(3) 0.049(3) 0.034(3) 0.007(2) 0.019(2) 0.023(3)
N8 0.054(3) 0.050(3) 0.046(3) 0.008(3) 0.028(3) 0.022(3)
O1 0.060(3) 0.057(3) 0.034(2) 0.010(2) 0.022(2) 0.021(2)
O2 0.040(2) 0.062(3) 0.054(3) -0.002(2) 0.012(2) 0.013(2)
O3 0.057(3) 0.052(3) 0.036(2) 0.005(2) 0.019(2) 0.022(2)
O4 0.041(2) 0.045(3) 0.052(3) 0.006(2) 0.013(2) 0.017(2)
O5 0.274(13) 0.273(14) 0.273(15) 0.018(13) 0.033(13) 0.002(12)
Os1 0.04134(15) 0.04549(17) 0.03453(15) 0.00795(11) 0.01842(11) 0.01444(11)
Os2 0.04236(15) 0.04751(17) 0.03370(15) 0.00692(11) 0.01772(11) 0.02009(12)
P1 0.132(4) 0.234(6) 0.110(3) -0.003(4) 0.033(3) 0.066(4)
S1 0.115(2) 0.0565(14) 0.105(2) -0.0113(13) 0.0429(17) 0.0121(14)
S2 0.0830(15) 0.0622(13) 0.0879(16) 0.0239(11) 0.0346(13) 0.0383(12)
O6 0.21(3) 0.22(3) 0.22(3) 0.026(11) 0.097(14) 0.050(12)
_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
C1 O1 1.339(8) . ?
C1 C6 1.391(10) . ?
C1 C2 1.424(10) . ?
C2 C3 1.372(12) . ?
C2 H2A 0.9300 . ?
C3 C4 1.359(13) . ?
C3 H3A 0.9300 . ?
C4 C5 1.368(12) . ?
C4 H4A 0.9300 . ?
C5 C6 1.417(10) . ?
C5 H5A 0.9300 . ?
C6 C7 1.445(10) . ?
C7 N1 1.316(8) . ?
C7 H7A 0.9300 . ?
C8 N1 1.479(8) . ?
C8 C9 1.518(10) . ?
C8 C13 1.534(9) . ?
C8 H8A 0.9800 . ?
C9 C10 1.510(11) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.545(13) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.531(11) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.534(10) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 N2 1.497(8) . ?
C13 H13A 0.9800 . ?
C14 N2 1.293(9) . ?
C14 C15 1.452(10) . ?
C14 H14A 0.9300 . ?
C15 C16 1.409(10) . ?
C15 C20 1.415(11) . ?
C16 C17 1.368(12) . ?
C16 H16A 0.9300 . ?
C17 C18 1.372(14) . ?
C17 H17A 0.9300 . ?
C18 C19 1.398(13) . ?
C18 H18A 0.9300 . ?
C19 C20 1.413(10) . ?
C19 H19A 0.9300 . ?
C20 O2 1.319(9) . ?
C21 N3 1.304(10) . ?
C21 S1 1.692(9) . ?
C21 H21A 0.9300 . ?
C22 C23 1.351(11) . ?
C22 S1 1.696(11) . ?
C22 H22A 0.9300 . ?
C23 N3 1.403(10) . ?
C23 C24 1.486(12) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 O3 1.335(9) . ?
C25 C26 1.394(10) . ?
C25 C30 1.423(10) . ?
C26 C27 1.359(12) . ?
C26 H26A 0.9300 . ?
C27 C28 1.407(14) . ?
C27 H27A 0.9300 . ?
C28 C29 1.363(12) . ?
C28 H28A 0.9300 . ?
C29 C30 1.415(11) . ?
C29 H29A 0.9300 . ?
C30 C31 1.441(10) . ?
C31 N6 1.290(9) . ?
C31 H31A 0.9300 . ?
C32 N6 1.480(8) . ?
C32 C33 1.518(9) . ?
C32 C37 1.535(11) . ?
C32 H32A 0.9800 . ?
C33 C34 1.516(11) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 C35 1.515(14) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 C36 1.522(11) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 C37 1.513(10) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C37 N7 1.505(8) . ?
C37 H37A 0.9800 . ?
C38 N7 1.282(9) . ?
C38 C39 1.445(10) . ?
C38 H38A 0.9300 . ?
C39 C40 1.410(10) . ?
C39 C44 1.452(10) . ?
C40 C41 1.357(11) . ?
C40 H40A 0.9300 . ?
C41 C42 1.393(12) . ?
C41 H41A 0.9300 . ?
C42 C43 1.356(11) . ?
C42 H42A 0.9300 . ?
C43 C44 1.430(10) . ?
C43 H43A 0.9300 . ?
C44 O4 1.287(8) . ?
C45 N8 1.329(9) . ?
C45 S2 1.685(7) . ?
C45 H45A 0.9300 . ?
C46 C47 1.345(11) . ?
C46 S2 1.707(9) . ?
C46 H46A 0.9300 . ?
C47 N8 1.378(9) . ?
C47 C48 1.513(11) . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C49 C50 1.524(16) . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C50 O5 1.340(15) . ?
C50 H50A 0.9700 . ?
C50 H50B 0.9700 . ?
C51 O5 1.433(15) . ?
C51 C52 1.494(15) . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
F1 P1 1.449(13) . ?
F2 P1 1.547(18) . ?
F3 P1 1.613(12) . ?
F4 P1 1.573(18) . ?
F5 P1 1.515(12) . ?
F6 P1 1.495(18) . ?
N1 Os1 2.028(5) . ?
N2 Os1 2.024(5) . ?
N3 Os1 2.107(6) . ?
N4 N5 1.165(8) . ?
N4 Os1 1.883(6) . ?
N5 Os2 1.877(6) . ?
N6 Os2 2.031(5) . ?
N7 Os2 2.020(5) . ?
N8 Os2 2.116(6) . ?
O1 Os1 2.013(4) . ?
O2 Os1 2.034(5) . ?
O3 Os2 2.007(4) . ?
O4 Os2 2.030(4) . ?
O6 H6A 0.8916 . ?
O6 H6B 0.8838 . ?
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
O1 C1 C6 124.1(6) . . ?
O1 C1 C2 117.3(7) . . ?
C6 C1 C2 118.5(7) . . ?
C3 C2 C1 119.1(9) . . ?
C3 C2 H2A 120.4 . . ?
C1 C2 H2A 120.4 . . ?
C4 C3 C2 123.5(8) . . ?
C4 C3 H3A 118.3 . . ?
C2 C3 H3A 118.3 . . ?
C3 C4 C5 117.9(8) . . ?
C3 C4 H4A 121.1 . . ?
C5 C4 H4A 121.1 . . ?
C4 C5 C6 122.1(9) . . ?
C4 C5 H5A 119.0 . . ?
C6 C5 H5A 119.0 . . ?
C1 C6 C5 118.9(7) . . ?
C1 C6 C7 121.5(6) . . ?
C5 C6 C7 117.4(7) . . ?
N1 C7 C6 122.6(6) . . ?
N1 C7 H7A 118.7 . . ?
C6 C7 H7A 118.7 . . ?
N1 C8 C9 118.1(6) . . ?
N1 C8 C13 103.9(5) . . ?
C9 C8 C13 110.4(6) . . ?
N1 C8 H8A 108.0 . . ?
C9 C8 H8A 108.0 . . ?
C13 C8 H8A 108.0 . . ?
C10 C9 C8 109.5(6) . . ?
C10 C9 H9A 109.8 . . ?
C8 C9 H9A 109.8 . . ?
C10 C9 H9B 109.8 . . ?
C8 C9 H9B 109.8 . . ?
H9A C9 H9B 108.2 . . ?
C9 C10 C11 111.5(7) . . ?
C9 C10 H10A 109.3 . . ?
C11 C10 H10A 109.3 . . ?
C9 C10 H10B 109.3 . . ?
C11 C10 H10B 109.3 . . ?
H10A C10 H10B 108.0 . . ?
C12 C11 C10 112.0(7) . . ?
C12 C11 H11A 109.2 . . ?
C10 C11 H11A 109.2 . . ?
C12 C11 H11B 109.2 . . ?
C10 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
C11 C12 C13 110.5(7) . . ?
C11 C12 H12A 109.5 . . ?
C13 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C13 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
N2 C13 C8 107.8(5) . . ?
N2 C13 C12 116.0(6) . . ?
C8 C13 C12 110.5(6) . . ?
N2 C13 H13A 107.4 . . ?
C8 C13 H13A 107.4 . . ?
C12 C13 H13A 107.4 . . ?
N2 C14 C15 125.3(7) . . ?
N2 C14 H14A 117.3 . . ?
C15 C14 H14A 117.3 . . ?
C16 C15 C20 119.2(7) . . ?
C16 C15 C14 114.5(7) . . ?
C20 C15 C14 126.3(6) . . ?
C17 C16 C15 121.9(9) . . ?
C17 C16 H16A 119.1 . . ?
C15 C16 H16A 119.1 . . ?
C16 C17 C18 120.0(8) . . ?
C16 C17 H17A 120.0 . . ?
C18 C17 H17A 120.0 . . ?
C17 C18 C19 120.0(8) . . ?
C17 C18 H18A 120.0 . . ?
C19 C18 H18A 120.0 . . ?
C18 C19 C20 121.5(9) . . ?
C18 C19 H19A 119.2 . . ?
C20 C19 H19A 119.2 . . ?
O2 C20 C19 116.1(7) . . ?
O2 C20 C15 126.5(6) . . ?
C19 C20 C15 117.4(7) . . ?
N3 C21 S1 115.5(7) . . ?
N3 C21 H21A 122.3 . . ?
S1 C21 H21A 122.3 . . ?
C23 C22 S1 111.6(7) . . ?
C23 C22 H22A 124.2 . . ?
S1 C22 H22A 124.2 . . ?
C22 C23 N3 113.1(8) . . ?
C22 C23 C24 125.2(8) . . ?
N3 C23 C24 121.7(7) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O3 C25 C26 118.6(7) . . ?
O3 C25 C30 123.4(6) . . ?
C26 C25 C30 117.8(7) . . ?
C27 C26 C25 122.7(9) . . ?
C27 C26 H26A 118.6 . . ?
C25 C26 H26A 118.6 . . ?
C26 C27 C28 120.2(8) . . ?
C26 C27 H27A 119.9 . . ?
C28 C27 H27A 119.9 . . ?
C29 C28 C27 118.7(9) . . ?
C29 C28 H28A 120.7 . . ?
C27 C28 H28A 120.7 . . ?
C28 C29 C30 122.2(9) . . ?
C28 C29 H29A 118.9 . . ?
C30 C29 H29A 118.9 . . ?
C29 C30 C25 118.4(7) . . ?
C29 C30 C31 118.7(7) . . ?
C25 C30 C31 121.1(7) . . ?
N6 C31 C30 123.5(6) . . ?
N6 C31 H31A 118.2 . . ?
C30 C31 H31A 118.2 . . ?
N6 C32 C33 118.4(6) . . ?
N6 C32 C37 104.6(5) . . ?
C33 C32 C37 110.1(6) . . ?
N6 C32 H32A 107.8 . . ?
C33 C32 H32A 107.8 . . ?
C37 C32 H32A 107.8 . . ?
C32 C33 C34 108.9(6) . . ?
C32 C33 H33A 109.9 . . ?
C34 C33 H33A 109.9 . . ?
C32 C33 H33B 109.9 . . ?
C34 C33 H33B 109.9 . . ?
H33A C33 H33B 108.3 . . ?
C33 C34 C35 111.3(7) . . ?
C33 C34 H34A 109.4 . . ?
C35 C34 H34A 109.4 . . ?
C33 C34 H34B 109.4 . . ?
C35 C34 H34B 109.4 . . ?
H34A C34 H34B 108.0 . . ?
C34 C35 C36 113.0(7) . . ?
C34 C35 H35A 109.0 . . ?
C36 C35 H35A 109.0 . . ?
C34 C35 H35B 109.0 . . ?
C36 C35 H35B 109.0 . . ?
H35A C35 H35B 107.8 . . ?
C37 C36 C35 110.3(7) . . ?
C37 C36 H36A 109.6 . . ?
C35 C36 H36A 109.6 . . ?
C37 C36 H36B 109.6 . . ?
C35 C36 H36B 109.6 . . ?
H36A C36 H36B 108.1 . . ?
N7 C37 C36 116.2(6) . . ?
N7 C37 C32 107.3(5) . . ?
C36 C37 C32 111.7(6) . . ?
N7 C37 H37A 107.1 . . ?
C36 C37 H37A 107.1 . . ?
C32 C37 H37A 107.1 . . ?
N7 C38 C39 126.2(6) . . ?
N7 C38 H38A 116.9 . . ?
C39 C38 H38A 116.9 . . ?
C40 C39 C38 116.6(6) . . ?
C40 C39 C44 118.1(6) . . ?
C38 C39 C44 125.3(6) . . ?
C41 C40 C39 123.6(7) . . ?
C41 C40 H40A 118.2 . . ?
C39 C40 H40A 118.2 . . ?
C40 C41 C42 118.2(7) . . ?
C40 C41 H41A 120.9 . . ?
C42 C41 H41A 120.9 . . ?
C43 C42 C41 121.8(7) . . ?
C43 C42 H42A 119.1 . . ?
C41 C42 H42A 119.1 . . ?
C42 C43 C44 122.1(8) . . ?
C42 C43 H43A 119.0 . . ?
C44 C43 H43A 119.0 . . ?
O4 C44 C43 118.1(6) . . ?
O4 C44 C39 125.7(6) . . ?
C43 C44 C39 116.2(7) . . ?
N8 C45 S2 114.6(6) . . ?
N8 C45 H45A 122.7 . . ?
S2 C45 H45A 122.7 . . ?
C47 C46 S2 111.7(7) . . ?
C47 C46 H46A 124.1 . . ?
S2 C46 H46A 124.1 . . ?
C46 C47 N8 113.4(7) . . ?
C46 C47 C48 124.8(8) . . ?
N8 C47 C48 121.8(7) . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C50 C49 H49A 109.5 . . ?
C50 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C50 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
O5 C50 C49 134(2) . . ?
O5 C50 H50A 103.8 . . ?
C49 C50 H50A 103.8 . . ?
O5 C50 H50B 103.8 . . ?
C49 C50 H50B 103.8 . . ?
H50A C50 H50B 105.4 . . ?
O5 C51 C52 116.2(13) . . ?
O5 C51 H51A 108.2 . . ?
C52 C51 H51A 108.2 . . ?
O5 C51 H51B 108.2 . . ?
C52 C51 H51B 108.2 . . ?
H51A C51 H51B 107.4 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C7 N1 C8 119.7(6) . . ?
C7 N1 Os1 125.6(5) . . ?
C8 N1 Os1 111.0(4) . . ?
C14 N2 C13 120.8(6) . . ?
C14 N2 Os1 124.2(5) . . ?
C13 N2 Os1 114.9(4) . . ?
C21 N3 C23 110.3(7) . . ?
C21 N3 Os1 120.5(6) . . ?
C23 N3 Os1 129.1(5) . . ?
N5 N4 Os1 178.9(5) . . ?
N4 N5 Os2 177.5(5) . . ?
C31 N6 C32 120.6(6) . . ?
C31 N6 Os2 126.3(5) . . ?
C32 N6 Os2 109.4(4) . . ?
C38 N7 C37 120.8(6) . . ?
C38 N7 Os2 124.3(5) . . ?
C37 N7 Os2 114.8(4) . . ?
C45 N8 C47 110.9(6) . . ?
C45 N8 Os2 119.0(5) . . ?
C47 N8 Os2 129.9(5) . . ?
C1 O1 Os1 121.7(4) . . ?
C20 O2 Os1 122.7(5) . . ?
C25 O3 Os2 122.2(4) . . ?
C44 O4 Os2 124.2(4) . . ?
C50 O5 C51 131.8(19) . . ?
N4 Os1 O1 177.0(2) . . ?
N4 Os1 N2 87.9(2) . . ?
O1 Os1 N2 94.8(2) . . ?
N4 Os1 N1 96.0(2) . . ?
O1 Os1 N1 85.9(2) . . ?
N2 Os1 N1 79.4(2) . . ?
N4 Os1 O2 92.4(2) . . ?
O1 Os1 O2 86.0(2) . . ?
N2 Os1 O2 94.3(2) . . ?
N1 Os1 O2 169.3(2) . . ?
N4 Os1 N3 91.4(2) . . ?
O1 Os1 N3 85.9(2) . . ?
N2 Os1 N3 179.1(2) . . ?
N1 Os1 N3 101.2(2) . . ?
O2 Os1 N3 85.1(2) . . ?
N5 Os2 O3 176.67(19) . . ?
N5 Os2 N7 87.9(2) . . ?
O3 Os2 N7 94.5(2) . . ?
N5 Os2 O4 92.0(2) . . ?
O3 Os2 O4 85.5(2) . . ?
N7 Os2 O4 94.0(2) . . ?
N5 Os2 N6 96.8(2) . . ?
O3 Os2 N6 86.0(2) . . ?
N7 Os2 N6 79.7(2) . . ?
O4 Os2 N6 168.9(2) . . ?
N5 Os2 N8 91.8(2) . . ?
O3 Os2 N8 85.8(2) . . ?
N7 Os2 N8 179.1(2) . . ?
O4 Os2 N8 85.2(2) . . ?
N6 Os2 N8 101.1(2) . . ?
F1 P1 F6 98.0(17) . . ?
F1 P1 F5 89.7(9) . . ?
F6 P1 F5 91.3(11) . . ?
F1 P1 F2 88.0(14) . . ?
F6 P1 F2 173.8(18) . . ?
F5 P1 F2 90.4(13) . . ?
F1 P1 F4 170.8(17) . . ?
F6 P1 F4 91.2(15) . . ?
F5 P1 F4 90.6(9) . . ?
F2 P1 F4 82.8(16) . . ?
F1 P1 F3 89.6(9) . . ?
F6 P1 F3 85.3(10) . . ?
F5 P1 F3 176.3(10) . . ?
F2 P1 F3 93.2(12) . . ?
F4 P1 F3 90.7(9) . . ?
C21 S1 C22 89.6(4) . . ?
C45 S2 C46 89.4(4) . . ?
H6A O6 H6B 109.2 . . ?
_diffrn_measured_fraction_theta_max 0.976
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.976
_refine_diff_density_max 1.451
_refine_diff_density_min -1.359
_refine_diff_density_rms 0.140
#==============================================================================
data_15
_database_code_depnum_ccdc_archive 'CCDC 777082'
#TrackingRef '- ALL.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C58 H66 N8 O4 Os2, 2(F6 P)'
_chemical_formula_sum 'C58 H66 F12 N8 O4 Os2 P2'
_chemical_formula_weight 1609.53
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -1.2165 7.6030 '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 15.1514(6)
_cell_length_b 12.7927(5)
_cell_length_c 17.8244(7)
_cell_angle_alpha 90.00
_cell_angle_beta 114.3590(10)
_cell_angle_gamma 90.00
_cell_volume 3147.3(2)
_cell_formula_units_Z 2
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 9201
_cell_measurement_theta_min 2.51
_cell_measurement_theta_max 28.28
_exptl_crystal_description plate
_exptl_crystal_colour dark-red
_exptl_crystal_size_max 0.26
_exptl_crystal_size_mid 0.16
_exptl_crystal_size_min 0.14
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.698
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1584
_exptl_absorpt_coefficient_mu 4.171
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.8229
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_process_details ?
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 293(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 'Smart CCD'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 18442
_diffrn_reflns_av_R_equivalents 0.0241
_diffrn_reflns_av_sigmaI/netI 0.0300
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_theta_min 2.03
_diffrn_reflns_theta_max 28.28
_reflns_number_total 7309
_reflns_number_gt 6028
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'SMART (Bruker, 1998)'
_computing_cell_refinement 'SAINT (Bruker, 1999)'
_computing_data_reduction SAINT
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_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.
The disorder of the t-Bu group was resolved into
two partial-occupancy orientations and the occupancy factors were
refined to 0.546(10) and 0.454(10). Two sites of these atoms were
refined with C23---C26 = C23---C26' = 1.55(2) \%A
and SIMU = 0.01 restraint.
;
_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^)+(0.0307P)^2^+1.8306P] 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 7309
_refine_ls_number_parameters 425
_refine_ls_number_restraints 32
_refine_ls_R_factor_all 0.0374
_refine_ls_R_factor_gt 0.0260
_refine_ls_wR_factor_ref 0.0681
_refine_ls_wR_factor_gt 0.0622
_refine_ls_goodness_of_fit_ref 1.053
_refine_ls_restrained_S_all 1.057
_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
C1 C 0.3724(2) 0.4361(3) 1.0934(2) 0.0461(8) Uani 1 1 d . . .
C2 C 0.4632(3) 0.4770(3) 1.1068(3) 0.0580(10) Uani 1 1 d . . .
H2A H 0.4832 0.5402 1.1345 0.070 Uiso 1 1 calc R . .
C3 C 0.5232(3) 0.4236(4) 1.0791(3) 0.0726(12) Uani 1 1 d . . .
H3A H 0.5827 0.4526 1.0871 0.087 Uiso 1 1 calc R . .
C4 C 0.4969(3) 0.3284(4) 1.0398(3) 0.0758(13) Uani 1 1 d . . .
H4A H 0.5383 0.2938 1.0215 0.091 Uiso 1 1 calc R . .
C5 C 0.4101(3) 0.2854(3) 1.0279(3) 0.0630(10) Uani 1 1 d . . .
H5A H 0.3936 0.2199 1.0035 0.076 Uiso 1 1 calc R . .
C6 C 0.3447(3) 0.3390(3) 1.0522(2) 0.0496(8) Uani 1 1 d . . .
C7 C 0.2601(3) 0.2849(3) 1.0487(2) 0.0510(9) Uani 1 1 d . . .
H7A H 0.2574 0.2127 1.0417 0.061 Uiso 1 1 calc R . .
C8 C 0.1215(3) 0.2747(3) 1.0830(2) 0.0474(8) Uani 1 1 d . . .
H8A H 0.0551 0.2974 1.0490 0.057 Uiso 1 1 calc R . .
C9 C 0.1235(3) 0.1565(3) 1.0815(3) 0.0671(11) Uani 1 1 d . . .
H9A H 0.1879 0.1314 1.1163 0.081 Uiso 1 1 calc R . .
H9B H 0.1070 0.1321 1.0258 0.081 Uiso 1 1 calc R . .
C10 C 0.0504(4) 0.1150(3) 1.1125(3) 0.0833(15) Uani 1 1 d . . .
H10A H -0.0140 0.1387 1.0765 0.100 Uiso 1 1 calc R . .
H10B H 0.0506 0.0392 1.1115 0.100 Uiso 1 1 calc R . .
C11 C 0.0751(4) 0.1524(4) 1.1993(4) 0.0842(15) Uani 1 1 d . . .
H11A H 0.1373 0.1238 1.2359 0.101 Uiso 1 1 calc R . .
H11B H 0.0267 0.1265 1.2173 0.101 Uiso 1 1 calc R . .
C12 C 0.0791(3) 0.2719(3) 1.2056(3) 0.0688(11) Uani 1 1 d . . .
H12A H 0.0149 0.3006 1.1749 0.083 Uiso 1 1 calc R . .
H12B H 0.1004 0.2927 1.2628 0.083 Uiso 1 1 calc R . .
C13 C 0.1490(3) 0.3155(3) 1.1713(2) 0.0500(9) Uani 1 1 d . . .
H13A H 0.2142 0.2903 1.2061 0.060 Uiso 1 1 calc R . .
C14 C 0.1265(3) 0.4919(3) 1.2123(2) 0.0501(9) Uani 1 1 d . . .
H14A H 0.1142 0.4596 1.2538 0.060 Uiso 1 1 calc R . .
C15 C 0.1141(3) 0.6035(3) 1.2051(2) 0.0475(8) Uani 1 1 d . . .
C16 C 0.0697(3) 0.6496(3) 1.2532(2) 0.0579(10) Uani 1 1 d . . .
H16A H 0.0555 0.6080 1.2895 0.069 Uiso 1 1 calc R . .
C17 C 0.0472(3) 0.7539(4) 1.2475(3) 0.0661(11) Uani 1 1 d . . .
H17A H 0.0161 0.7821 1.2782 0.079 Uiso 1 1 calc R . .
C18 C 0.0715(3) 0.8168(3) 1.1956(3) 0.0687(12) Uani 1 1 d . . .
H18A H 0.0573 0.8879 1.1923 0.082 Uiso 1 1 calc R . .
C19 C 0.1160(3) 0.7762(3) 1.1492(3) 0.0594(10) Uani 1 1 d . . .
H19A H 0.1323 0.8202 1.1153 0.071 Uiso 1 1 calc R . .
C20 C 0.1375(3) 0.6688(3) 1.1516(2) 0.0454(8) Uani 1 1 d . . .
C21 C 0.2315(3) 0.6327(3) 0.9619(2) 0.0511(9) Uani 1 1 d . . .
H21A H 0.2584 0.6712 1.0104 0.061 Uiso 1 1 calc R . .
C22 C 0.2349(3) 0.6731(3) 0.8921(2) 0.0590(10) Uani 1 1 d . A .
H22A H 0.2643 0.7376 0.8946 0.071 Uiso 1 1 calc R . .
C23 C 0.1955(3) 0.6204(3) 0.8180(2) 0.0554(9) Uani 1 1 d D . .
C24 C 0.1552(4) 0.5246(3) 0.8205(3) 0.0659(11) Uani 1 1 d . A .
H24A H 0.1282 0.4849 0.7727 0.079 Uiso 1 1 calc R . .
C25 C 0.1540(3) 0.4866(3) 0.8918(2) 0.0564(10) Uani 1 1 d . . .
H25A H 0.1264 0.4214 0.8909 0.068 Uiso 1 1 calc R A .
C26 C 0.2064(15) 0.673(2) 0.7444(9) 0.061(4) Uani 0.546(10) 1 d PD A 1
C27 C 0.0946(13) 0.6847(18) 0.6817(9) 0.147(6) Uani 0.546(10) 1 d PU A 1
H27A H 0.0905 0.7144 0.6308 0.220 Uiso 0.546(10) 1 calc PR A 1
H27B H 0.0621 0.7295 0.7054 0.220 Uiso 0.546(10) 1 calc PR A 1
H27C H 0.0644 0.6171 0.6713 0.220 Uiso 0.546(10) 1 calc PR A 1
C28 C 0.2596(15) 0.7697(12) 0.7575(10) 0.143(7) Uani 0.546(10) 1 d PU A 1
H28A H 0.2611 0.7923 0.7067 0.215 Uiso 0.546(10) 1 calc PR A 1
H28B H 0.3246 0.7591 0.7978 0.215 Uiso 0.546(10) 1 calc PR A 1
H28C H 0.2286 0.8221 0.7768 0.215 Uiso 0.546(10) 1 calc PR A 1
C29 C 0.2502(13) 0.5929(12) 0.7069(8) 0.123(4) Uani 0.546(10) 1 d PU A 1
H29A H 0.2522 0.6210 0.6577 0.184 Uiso 0.546(10) 1 calc PR A 1
H29B H 0.2113 0.5307 0.6937 0.184 Uiso 0.546(10) 1 calc PR A 1
H29C H 0.3147 0.5764 0.7456 0.184 Uiso 0.546(10) 1 calc PR A 1
C26' C 0.1786(18) 0.657(3) 0.7309(10) 0.058(5) Uani 0.454(10) 1 d PD A 2
C27' C 0.1479(19) 0.5876(15) 0.6638(9) 0.143(6) Uani 0.454(10) 1 d PU A 2
H27D H 0.1714 0.5187 0.6831 0.214 Uiso 0.454(10) 1 calc PR A 2
H27E H 0.1729 0.6100 0.6250 0.214 Uiso 0.454(10) 1 calc PR A 2
H27F H 0.0784 0.5867 0.6376 0.214 Uiso 0.454(10) 1 calc PR A 2
C28' C 0.1232(15) 0.7616(14) 0.7146(10) 0.111(6) Uani 0.454(10) 1 d PU A 2
H28D H 0.0760 0.7591 0.7375 0.167 Uiso 0.454(10) 1 calc PR A 2
H28E H 0.0912 0.7734 0.6563 0.167 Uiso 0.454(10) 1 calc PR A 2
H28F H 0.1679 0.8176 0.7398 0.167 Uiso 0.454(10) 1 calc PR A 2
C29' C 0.2831(17) 0.698(2) 0.7450(13) 0.142(6) Uani 0.454(10) 1 d PU A 2
H29D H 0.3262 0.6400 0.7541 0.213 Uiso 0.454(10) 1 calc PR A 2
H29E H 0.3073 0.7436 0.7921 0.213 Uiso 0.454(10) 1 calc PR A 2
H29F H 0.2790 0.7363 0.6972 0.213 Uiso 0.454(10) 1 calc PR A 2
F1 F 0.2683(4) 0.9646(4) 0.0975(3) 0.1501(16) Uani 1 1 d . . .
F2 F 0.3480(3) 0.8318(3) 0.0704(3) 0.1543(17) Uani 1 1 d . . .
F3 F 0.2096(3) 0.8815(3) -0.0203(3) 0.1653(19) Uani 1 1 d . . .
F4 F 0.4020(5) 0.9909(5) 0.0870(5) 0.246(4) Uani 1 1 d . . .
F5 F 0.3417(5) 0.9126(4) -0.0363(3) 0.199(2) Uani 1 1 d . . .
F6 F 0.2614(5) 1.0440(3) -0.0119(4) 0.197(3) Uani 1 1 d . . .
N1 N 0.1527(2) 0.4326(2) 1.16733(17) 0.0432(6) Uani 1 1 d . A .
N2 N 0.1873(2) 0.3315(2) 1.05482(17) 0.0436(6) Uani 1 1 d . A .
N3 N 0.0412(2) 0.49455(19) 1.01520(18) 0.0396(6) Uani 1 1 d . . .
N4 N 0.1912(2) 0.5400(2) 0.96338(17) 0.0420(6) Uani 1 1 d . A .
O1 O 0.31872(18) 0.48731(17) 1.12474(16) 0.0457(6) Uani 1 1 d . A .
O2 O 0.17989(18) 0.63716(17) 1.10411(15) 0.0488(6) Uani 1 1 d . A .
Os1 Os 0.175877(9) 0.487069(9) 1.069501(8) 0.03741(5) Uani 1 1 d . . .
P1 P 0.30670(14) 0.93841(11) 0.02923(10) 0.0951(5) 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
C1 0.0454(19) 0.053(2) 0.0381(18) 0.0039(15) 0.0156(15) 0.0029(15)
C2 0.050(2) 0.070(3) 0.054(2) -0.0018(18) 0.0207(18) -0.0043(18)
C3 0.050(2) 0.096(4) 0.080(3) 0.002(3) 0.035(2) -0.001(2)
C4 0.068(3) 0.095(4) 0.078(3) 0.000(3) 0.045(2) 0.015(3)
C5 0.068(3) 0.066(3) 0.061(3) -0.0047(19) 0.032(2) 0.011(2)
C6 0.051(2) 0.053(2) 0.046(2) 0.0026(15) 0.0205(16) 0.0071(16)
C7 0.058(2) 0.0421(19) 0.053(2) -0.0030(15) 0.0223(17) 0.0040(16)
C8 0.047(2) 0.0388(18) 0.054(2) 0.0068(15) 0.0181(16) -0.0016(14)
C9 0.074(3) 0.039(2) 0.088(3) 0.0048(19) 0.033(2) -0.0024(18)
C10 0.094(4) 0.047(2) 0.113(4) 0.012(3) 0.046(3) -0.014(2)
C11 0.098(4) 0.060(3) 0.108(4) 0.025(3) 0.055(3) -0.003(2)
C12 0.085(3) 0.060(2) 0.075(3) 0.015(2) 0.046(2) -0.004(2)
C13 0.054(2) 0.0436(19) 0.051(2) 0.0137(15) 0.0207(17) 0.0048(15)
C14 0.057(2) 0.055(2) 0.0406(19) 0.0067(15) 0.0226(17) -0.0008(16)
C15 0.053(2) 0.054(2) 0.0378(18) -0.0011(15) 0.0213(16) -0.0005(16)
C16 0.068(3) 0.066(3) 0.046(2) -0.0063(18) 0.0290(19) -0.0021(19)
C17 0.078(3) 0.072(3) 0.059(3) -0.015(2) 0.038(2) 0.006(2)
C18 0.088(3) 0.051(2) 0.072(3) -0.005(2) 0.038(2) 0.013(2)
C19 0.079(3) 0.046(2) 0.060(2) -0.0004(17) 0.036(2) 0.0050(19)
C20 0.050(2) 0.0470(19) 0.0392(18) -0.0056(14) 0.0182(15) 0.0002(15)
C21 0.064(2) 0.048(2) 0.049(2) -0.0059(15) 0.0314(18) -0.0092(17)
C22 0.080(3) 0.050(2) 0.062(3) 0.0021(18) 0.045(2) -0.0085(19)
C23 0.062(2) 0.063(2) 0.049(2) 0.0075(17) 0.0302(18) 0.0080(18)
C24 0.084(3) 0.075(3) 0.040(2) -0.0075(19) 0.028(2) -0.011(2)
C25 0.072(3) 0.052(2) 0.047(2) -0.0082(16) 0.026(2) -0.0138(18)
C26 0.055(12) 0.091(9) 0.041(6) 0.001(6) 0.024(6) -0.024(8)
C27 0.158(11) 0.209(14) 0.083(9) 0.077(10) 0.059(8) 0.036(12)
C28 0.230(15) 0.120(11) 0.104(9) 0.035(9) 0.093(9) -0.057(12)
C29 0.192(11) 0.140(9) 0.081(7) 0.009(7) 0.101(7) 0.016(10)
C26' 0.041(11) 0.091(14) 0.040(7) 0.013(8) 0.015(6) -0.015(8)
C27' 0.230(14) 0.152(12) 0.055(7) 0.019(8) 0.067(8) -0.001(12)
C28' 0.151(13) 0.122(12) 0.086(10) 0.065(9) 0.074(10) 0.057(11)
C29' 0.177(12) 0.174(14) 0.103(10) 0.053(12) 0.086(9) -0.008(14)
F1 0.196(5) 0.168(4) 0.107(3) -0.004(3) 0.083(3) 0.034(3)
F2 0.157(4) 0.099(3) 0.164(4) 0.020(3) 0.023(3) 0.009(2)
F3 0.121(3) 0.136(4) 0.190(4) -0.050(3) 0.015(3) 0.014(3)
F4 0.213(6) 0.216(6) 0.336(10) -0.188(6) 0.140(7) -0.124(5)
F5 0.367(8) 0.124(4) 0.211(5) -0.024(3) 0.226(5) -0.002(4)
F6 0.396(9) 0.076(2) 0.190(5) 0.020(3) 0.190(6) 0.047(4)
N1 0.0466(16) 0.0416(15) 0.0398(15) 0.0080(12) 0.0160(12) 0.0026(12)
N2 0.0455(16) 0.0382(15) 0.0461(17) 0.0000(11) 0.0178(13) 0.0007(11)
N3 0.0452(14) 0.0371(14) 0.0387(15) 0.0064(11) 0.0196(12) 0.0028(12)
N4 0.0473(16) 0.0404(15) 0.0388(15) 0.0003(11) 0.0184(12) 0.0019(12)
O1 0.0406(13) 0.0493(13) 0.0462(14) -0.0065(10) 0.0167(11) -0.0020(10)
O2 0.0659(16) 0.0373(12) 0.0528(15) -0.0011(10) 0.0343(12) -0.0014(11)
Os1 0.04124(8) 0.03548(8) 0.03613(8) 0.00256(5) 0.01656(6) 0.00168(5)
P1 0.1564(15) 0.0525(7) 0.0934(11) -0.0195(7) 0.0687(11) -0.0148(8)
_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
C1 O1 1.334(4) . ?
C1 C2 1.397(5) . ?
C1 C6 1.415(5) . ?
C2 C3 1.381(6) . ?
C2 H2A 0.9300 . ?
C3 C4 1.380(7) . ?
C3 H3A 0.9300 . ?
C4 C5 1.358(6) . ?
C4 H4A 0.9300 . ?
C5 C6 1.412(5) . ?
C5 H5A 0.9300 . ?
C6 C7 1.435(5) . ?
C7 N2 1.297(4) . ?
C7 H7A 0.9300 . ?
C8 N2 1.480(4) . ?
C8 C9 1.513(5) . ?
C8 C13 1.543(5) . ?
C8 H8A 0.9800 . ?
C9 C10 1.523(6) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.512(7) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.533(6) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.529(5) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 N1 1.502(4) . ?
C13 H13A 0.9800 . ?
C14 N1 1.280(5) . ?
C14 C15 1.439(5) . ?
C14 H14A 0.9300 . ?
C15 C16 1.418(5) . ?
C15 C20 1.419(5) . ?
C16 C17 1.371(6) . ?
C16 H16A 0.9300 . ?
C17 C18 1.385(6) . ?
C17 H17A 0.9300 . ?
C18 C19 1.368(6) . ?
C18 H18A 0.9300 . ?
C19 C20 1.408(5) . ?
C19 H19A 0.9300 . ?
C20 O2 1.319(4) . ?
C21 N4 1.338(4) . ?
C21 C22 1.368(5) . ?
C21 H21A 0.9300 . ?
C22 C23 1.380(5) . ?
C22 H22A 0.9300 . ?
C23 C24 1.378(6) . ?
C23 C26 1.544(14) . ?
C23 C26' 1.538(15) . ?
C24 C25 1.368(6) . ?
C24 H24A 0.9300 . ?
C25 N4 1.348(5) . ?
C25 H25A 0.9300 . ?
C26 C27 1.61(2) . ?
C26 C28 1.44(2) . ?
C26 C29 1.52(4) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C26' C29' 1.59(3) . ?
C26' C27' 1.41(3) . ?
C26' C28' 1.54(4) . ?
C27' H27D 0.9600 . ?
C27' H27E 0.9600 . ?
C27' H27F 0.9600 . ?
C28' H28D 0.9600 . ?
C28' H28E 0.9600 . ?
C28' H28F 0.9600 . ?
C29' H29D 0.9600 . ?
C29' H29E 0.9600 . ?
C29' H29F 0.9600 . ?
F1 P1 1.586(4) . ?
F2 P1 1.554(4) . ?
F3 P1 1.549(4) . ?
F4 P1 1.539(6) . ?
F5 P1 1.505(4) . ?
F6 P1 1.555(5) . ?
N1 Os1 2.038(3) . ?
N2 Os1 2.025(3) . ?
N3 N3 1.146(6) 3_567 ?
N3 Os1 1.866(3) . ?
N4 Os1 2.110(3) . ?
O1 Os1 1.974(2) . ?
O2 Os1 2.010(2) . ?
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
O1 C1 C2 118.1(3) . . ?
O1 C1 C6 123.1(3) . . ?
C2 C1 C6 118.6(3) . . ?
C3 C2 C1 120.0(4) . . ?
C3 C2 H2A 120.0 . . ?
C1 C2 H2A 120.0 . . ?
C4 C3 C2 121.5(4) . . ?
C4 C3 H3A 119.2 . . ?
C2 C3 H3A 119.2 . . ?
C5 C4 C3 119.7(4) . . ?
C5 C4 H4A 120.2 . . ?
C3 C4 H4A 120.2 . . ?
C4 C5 C6 120.8(4) . . ?
C4 C5 H5A 119.6 . . ?
C6 C5 H5A 119.6 . . ?
C5 C6 C1 119.3(4) . . ?
C5 C6 C7 118.6(4) . . ?
C1 C6 C7 121.0(3) . . ?
N2 C7 C6 123.3(3) . . ?
N2 C7 H7A 118.3 . . ?
C6 C7 H7A 118.3 . . ?
N2 C8 C9 117.6(3) . . ?
N2 C8 C13 104.2(3) . . ?
C9 C8 C13 111.0(3) . . ?
N2 C8 H8A 107.9 . . ?
C9 C8 H8A 107.9 . . ?
C13 C8 H8A 107.9 . . ?
C8 C9 C10 108.6(4) . . ?
C8 C9 H9A 110.0 . . ?
C10 C9 H9A 110.0 . . ?
C8 C9 H9B 110.0 . . ?
C10 C9 H9B 110.0 . . ?
H9A C9 H9B 108.4 . . ?
C11 C10 C9 110.6(4) . . ?
C11 C10 H10A 109.5 . . ?
C9 C10 H10A 109.5 . . ?
C11 C10 H10B 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
C10 C11 C12 112.1(4) . . ?
C10 C11 H11A 109.2 . . ?
C12 C11 H11A 109.2 . . ?
C10 C11 H11B 109.2 . . ?
C12 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
C13 C12 C11 110.4(4) . . ?
C13 C12 H12A 109.6 . . ?
C11 C12 H12A 109.6 . . ?
C13 C12 H12B 109.6 . . ?
C11 C12 H12B 109.6 . . ?
H12A C12 H12B 108.1 . . ?
N1 C13 C12 115.4(3) . . ?
N1 C13 C8 106.8(3) . . ?
C12 C13 C8 110.1(3) . . ?
N1 C13 H13A 108.1 . . ?
C12 C13 H13A 108.1 . . ?
C8 C13 H13A 108.1 . . ?
N1 C14 C15 126.5(3) . . ?
N1 C14 H14A 116.8 . . ?
C15 C14 H14A 116.8 . . ?
C16 C15 C20 118.3(3) . . ?
C16 C15 C14 115.8(3) . . ?
C20 C15 C14 125.8(3) . . ?
C17 C16 C15 121.7(4) . . ?
C17 C16 H16A 119.1 . . ?
C15 C16 H16A 119.1 . . ?
C16 C17 C18 119.2(4) . . ?
C16 C17 H17A 120.4 . . ?
C18 C17 H17A 120.4 . . ?
C19 C18 C17 121.0(4) . . ?
C19 C18 H18A 119.5 . . ?
C17 C18 H18A 119.5 . . ?
C18 C19 C20 121.2(4) . . ?
C18 C19 H19A 119.4 . . ?
C20 C19 H19A 119.4 . . ?
O2 C20 C19 116.6(3) . . ?
O2 C20 C15 125.0(3) . . ?
C19 C20 C15 118.4(3) . . ?
N4 C21 C22 122.7(3) . . ?
N4 C21 H21A 118.6 . . ?
C22 C21 H21A 118.6 . . ?
C21 C22 C23 121.5(4) . . ?
C21 C22 H22A 119.2 . . ?
C23 C22 H22A 119.2 . . ?
C24 C23 C22 115.2(3) . . ?
C24 C23 C26 128.4(10) . . ?
C22 C23 C26 116.4(9) . . ?
C24 C23 C26' 114.4(10) . . ?
C22 C23 C26' 130.0(12) . . ?
C26 C23 C26' 16.4(9) . . ?
C25 C24 C23 121.5(4) . . ?
C25 C24 H24A 119.3 . . ?
C23 C24 H24A 119.3 . . ?
N4 C25 C24 122.5(4) . . ?
N4 C25 H25A 118.7 . . ?
C24 C25 H25A 118.7 . . ?
C27 C26 C28 113(2) . . ?
C27 C26 C23 100.4(11) . . ?
C28 C26 C23 119.0(14) . . ?
C27 C26 C29 106.4(15) . . ?
C28 C26 C29 109.5(15) . . ?
C23 C26 C29 107.3(19) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C29' C26' C27' 108(2) . . ?
C29' C26' C23 101.7(12) . . ?
C27' C26' C23 122(2) . . ?
C29' C26' C28' 99.9(19) . . ?
C27' C26' C28' 115.1(17) . . ?
C23 C26' C28' 108(2) . . ?
C26' C27' H27D 109.5 . . ?
C26' C27' H27E 109.5 . . ?
H27D C27' H27E 109.5 . . ?
C26' C27' H27F 109.5 . . ?
H27D C27' H27F 109.5 . . ?
H27E C27' H27F 109.5 . . ?
C26' C28' H28D 109.5 . . ?
C26' C28' H28E 109.5 . . ?
H28D C28' H28E 109.5 . . ?
C26' C28' H28F 109.5 . . ?
H28D C28' H28F 109.5 . . ?
H28E C28' H28F 109.5 . . ?
C26' C29' H29D 109.5 . . ?
C26' C29' H29E 109.5 . . ?
H29D C29' H29E 109.5 . . ?
C26' C29' H29F 109.5 . . ?
H29D C29' H29F 109.5 . . ?
H29E C29' H29F 109.5 . . ?
C14 N1 C13 122.3(3) . . ?
C14 N1 Os1 122.8(2) . . ?
C13 N1 Os1 113.9(2) . . ?
C7 N2 C8 121.3(3) . . ?
C7 N2 Os1 125.7(2) . . ?
C8 N2 Os1 109.4(2) . . ?
N3 N3 Os1 175.2(4) 3_567 . ?
C21 N4 C25 116.6(3) . . ?
C21 N4 Os1 121.4(2) . . ?
C25 N4 Os1 121.8(2) . . ?
C1 O1 Os1 121.5(2) . . ?
C20 O2 Os1 121.9(2) . . ?
N3 Os1 O1 176.73(10) . . ?
N3 Os1 O2 89.91(10) . . ?
O1 Os1 O2 87.55(10) . . ?
N3 Os1 N2 96.73(11) . . ?
O1 Os1 N2 86.05(10) . . ?
O2 Os1 N2 170.27(10) . . ?
N3 Os1 N1 85.62(11) . . ?
O1 Os1 N1 96.57(11) . . ?
O2 Os1 N1 93.33(11) . . ?
N2 Os1 N1 80.14(12) . . ?
N3 Os1 N4 91.13(11) . . ?
O1 Os1 N4 86.74(11) . . ?
O2 Os1 N4 88.16(10) . . ?
N2 Os1 N4 98.78(11) . . ?
N1 Os1 N4 176.42(10) . . ?
F5 P1 F4 94.7(4) . . ?
F5 P1 F3 90.6(3) . . ?
F4 P1 F3 173.7(4) . . ?
F5 P1 F2 88.4(3) . . ?
F4 P1 F2 89.0(4) . . ?
F3 P1 F2 87.7(2) . . ?
F5 P1 F6 93.1(3) . . ?
F4 P1 F6 92.7(4) . . ?
F3 P1 F6 90.5(4) . . ?
F2 P1 F6 177.7(3) . . ?
F5 P1 F1 179.1(3) . . ?
F4 P1 F1 86.2(3) . . ?
F3 P1 F1 88.6(3) . . ?
F2 P1 F1 91.5(3) . . ?
F6 P1 F1 87.0(2) . . ?
_diffrn_measured_fraction_theta_max 0.936
_diffrn_reflns_theta_full 28.28
_diffrn_measured_fraction_theta_full 0.936
_refine_diff_density_max 1.195
_refine_diff_density_min -0.479
_refine_diff_density_rms 0.083
#==============================================================================
data_16
_database_code_depnum_ccdc_archive 'CCDC 777083'
#TrackingRef '- ALL.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C48 H50 N8 O4 Os2 S2, 2(F6 P)'
_chemical_formula_sum 'C48 H50 F12 N8 O4 Os2 P2 S2'
_chemical_formula_weight 1537.42
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -1.2165 7.6030 '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 12.1740(10)
_cell_length_b 20.3147(16)
_cell_length_c 22.3730(18)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 5533.1(8)
_cell_formula_units_Z 4
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 5570
_cell_measurement_theta_min 2.15
_cell_measurement_theta_max 22.85
_exptl_crystal_description needle
_exptl_crystal_colour dark-red
_exptl_crystal_size_max 0.40
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.08
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.846
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 2992
_exptl_absorpt_coefficient_mu 4.813
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.7913
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_process_details ?
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 293(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 'Smart CCD'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 26024
_diffrn_reflns_av_R_equivalents 0.0584
_diffrn_reflns_av_sigmaI/netI 0.0459
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_k_min -22
_diffrn_reflns_limit_k_max 24
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_limit_l_max 26
_diffrn_reflns_theta_min 2.00
_diffrn_reflns_theta_max 24.99
_reflns_number_total 4864
_reflns_number_gt 3227
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'SMART (Bruker, 1998)'
_computing_cell_refinement 'SAINT (Bruker, 1999)'
_computing_data_reduction SAINT
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_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.
The atoms C10, C9, C13, C4, S1, N4, C23, C21, C22, of the structure
were refined with SIMU = 0.01 restraint.
;
_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^)+(0.0503P)^2^+22.7683P] 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 4864
_refine_ls_number_parameters 352
_refine_ls_number_restraints 36
_refine_ls_R_factor_all 0.0846
_refine_ls_R_factor_gt 0.0486
_refine_ls_wR_factor_ref 0.1272
_refine_ls_wR_factor_gt 0.1108
_refine_ls_goodness_of_fit_ref 1.098
_refine_ls_restrained_S_all 1.119
_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
C1 C 0.1636(11) 0.0915(8) 0.3036(5) 0.093(5) Uani 1 1 d . . .
C2 C 0.1902(13) 0.1502(9) 0.2743(6) 0.131(6) Uani 1 1 d . . .
H2A H 0.1360 0.1818 0.2681 0.157 Uiso 1 1 calc R . .
C3 C 0.2919(18) 0.1614(14) 0.2551(8) 0.163(11) Uani 1 1 d . . .
H3A H 0.3087 0.2016 0.2374 0.195 Uiso 1 1 calc R . .
C4 C 0.3714(18) 0.1152(13) 0.2608(9) 0.159(12) Uani 1 1 d . . .
H4A H 0.4417 0.1243 0.2469 0.191 Uiso 1 1 calc R . .
C5 C 0.3498(12) 0.0533(10) 0.2877(7) 0.138(8) Uani 1 1 d . . .
H5A H 0.4035 0.0208 0.2902 0.165 Uiso 1 1 calc R . .
C6 C 0.2421(11) 0.0432(9) 0.3105(5) 0.090(4) Uani 1 1 d . . .
C7 C 0.2090(9) -0.0207(7) 0.3323(5) 0.078(4) Uani 1 1 d . . .
H7A H 0.2497 -0.0569 0.3197 0.094 Uiso 1 1 calc R . .
C8 C 0.0694(9) -0.0941(5) 0.3732(6) 0.069(3) Uani 1 1 d . . .
H8A H 0.0543 -0.1020 0.4156 0.083 Uiso 1 1 calc R . .
C9 C 0.1264(11) -0.1562(7) 0.3478(8) 0.121(5) Uani 1 1 d U . .
H9A H 0.1387 -0.1512 0.3052 0.146 Uiso 1 1 calc R . .
H9B H 0.1969 -0.1627 0.3671 0.146 Uiso 1 1 calc R . .
C10 C 0.0518(13) -0.2154(8) 0.3595(9) 0.132(5) Uani 1 1 d U . .
H10A H 0.0416 -0.2209 0.4022 0.158 Uiso 1 1 calc R . .
H10B H 0.0861 -0.2550 0.3441 0.158 Uiso 1 1 calc R . .
C11 C -0.0602(11) -0.2055(7) 0.3293(7) 0.109(5) Uani 1 1 d . . .
H11A H -0.0502 -0.2033 0.2863 0.131 Uiso 1 1 calc R . .
H11B H -0.1070 -0.2429 0.3380 0.131 Uiso 1 1 calc R . .
C12 C -0.1164(9) -0.1424(5) 0.3508(6) 0.083(4) Uani 1 1 d . . .
H12A H -0.1844 -0.1359 0.3290 0.099 Uiso 1 1 calc R . .
H12B H -0.1339 -0.1463 0.3929 0.099 Uiso 1 1 calc R . .
C13 C -0.0417(9) -0.0839(5) 0.3411(5) 0.064(3) Uani 1 1 d . . .
H13A H -0.0276 -0.0797 0.2982 0.077 Uiso 1 1 calc R . .
C14 C -0.1888(9) -0.0063(5) 0.3604(4) 0.056(3) Uani 1 1 d . . .
H14A H -0.2335 -0.0378 0.3427 0.068 Uiso 1 1 calc R . .
C15 C -0.2415(9) 0.0522(5) 0.3815(5) 0.062(3) Uani 1 1 d . . .
C16 C -0.3565(9) 0.0539(6) 0.3784(5) 0.076(3) Uani 1 1 d . . .
H16A H -0.3923 0.0187 0.3603 0.091 Uiso 1 1 calc R . .
C17 C -0.4181(10) 0.1035(7) 0.4002(6) 0.098(4) Uani 1 1 d . . .
H17A H -0.4943 0.1028 0.3977 0.118 Uiso 1 1 calc R . .
C18 C -0.3622(11) 0.1563(8) 0.4269(8) 0.119(5) Uani 1 1 d . . .
H18A H -0.4018 0.1908 0.4437 0.143 Uiso 1 1 calc R . .
C19 C -0.2514(11) 0.1573(7) 0.4283(8) 0.121(6) Uani 1 1 d . . .
H19A H -0.2164 0.1940 0.4443 0.145 Uiso 1 1 calc R . .
C20 C -0.1875(8) 0.1060(5) 0.4069(5) 0.068(3) Uani 1 1 d . . .
C21 C 0.1283(11) 0.1718(6) 0.4261(7) 0.101(2) Uani 1 1 d U . .
H21A H 0.0665 0.1881 0.4066 0.121 Uiso 1 1 calc R . .
C22 C 0.2945(11) 0.1548(7) 0.4795(7) 0.106(2) Uani 1 1 d U . .
H22A H 0.3592 0.1570 0.5014 0.127 Uiso 1 1 calc R . .
C23 C 0.2434(10) 0.0970(6) 0.4634(6) 0.089(2) Uani 1 1 d U . .
C24 C 0.2839(10) 0.0295(7) 0.4766(5) 0.100(5) Uani 1 1 d . . .
H24A H 0.2336 -0.0023 0.4605 0.150 Uiso 1 1 calc R . .
H24B H 0.2895 0.0237 0.5190 0.150 Uiso 1 1 calc R . .
H24C H 0.3549 0.0235 0.4587 0.150 Uiso 1 1 calc R . .
F1 F 0.6059(11) 0.8810(9) 0.3914(6) 0.233(7) Uani 1 1 d . . .
F2 F 0.4538(15) 0.9064(10) 0.3936(9) 0.299(11) Uani 1 1 d . . .
F3 F 0.485(2) 0.8104(9) 0.4129(9) 0.344(15) Uani 1 1 d . . .
F4 F 0.4098(11) 0.8332(12) 0.3285(10) 0.356(14) Uani 1 1 d . . .
F5 F 0.5626(16) 0.7966(9) 0.3301(9) 0.310(10) Uani 1 1 d . . .
F6 F 0.539(2) 0.8936(9) 0.3104(7) 0.334(14) Uani 1 1 d . . .
N1 N 0.1267(6) -0.0319(4) 0.3682(4) 0.062(2) Uani 1 1 d . . .
N2 N -0.0858(6) -0.0194(4) 0.3637(3) 0.053(2) Uani 1 1 d . . .
N3 N 0.0056(6) 0.0070(4) 0.4754(3) 0.0492(19) Uani 1 1 d . . .
N4 N 0.1459(8) 0.1081(5) 0.4333(5) 0.084(2) Uani 1 1 d U . .
O1 O 0.0599(6) 0.0847(4) 0.3223(3) 0.086(3) Uani 1 1 d . . .
O2 O -0.0795(6) 0.1129(4) 0.4137(4) 0.087(2) Uani 1 1 d . . .
Os1 Os 0.02914(3) 0.041303(18) 0.398898(15) 0.04767(15) Uani 1 1 d . . .
P1 P 0.5096(4) 0.8516(2) 0.3598(3) 0.1137(16) Uani 1 1 d . . .
S1 S 0.2255(3) 0.22094(19) 0.4547(2) 0.1217(14) Uani 1 1 d U . .
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
C1 0.052(8) 0.181(15) 0.046(6) 0.017(8) -0.002(6) -0.031(9)
C2 0.107(12) 0.190(17) 0.095(10) 0.052(11) 0.002(9) -0.084(12)
C3 0.131(18) 0.27(3) 0.091(12) -0.002(16) 0.035(13) -0.112(19)
C4 0.130(17) 0.24(3) 0.111(14) -0.095(16) 0.080(14) -0.125(18)
C5 0.063(9) 0.23(2) 0.124(13) -0.116(14) 0.040(9) -0.046(11)
C6 0.063(8) 0.164(14) 0.044(6) -0.033(8) 0.016(6) -0.042(9)
C7 0.035(6) 0.126(11) 0.074(7) -0.041(8) -0.007(6) 0.008(7)
C8 0.055(7) 0.069(7) 0.085(8) -0.011(6) -0.011(6) 0.002(6)
C9 0.087(9) 0.093(9) 0.183(12) -0.065(9) -0.022(9) 0.028(7)
C10 0.106(10) 0.091(9) 0.198(13) -0.050(10) -0.023(10) 0.034(7)
C11 0.095(11) 0.085(9) 0.147(13) -0.027(9) -0.020(10) -0.006(8)
C12 0.061(7) 0.073(8) 0.114(10) -0.012(7) -0.015(7) 0.003(6)
C13 0.065(7) 0.074(7) 0.054(6) -0.021(5) -0.005(5) 0.007(6)
C14 0.057(7) 0.058(6) 0.054(6) 0.002(5) -0.011(5) -0.007(5)
C15 0.050(6) 0.070(7) 0.067(6) 0.016(5) 0.001(5) -0.002(5)
C16 0.047(6) 0.090(9) 0.091(8) -0.004(7) -0.001(6) 0.009(6)
C17 0.041(6) 0.109(11) 0.144(13) -0.014(10) 0.004(8) 0.012(7)
C18 0.058(9) 0.107(11) 0.193(16) -0.046(11) 0.021(10) 0.018(8)
C19 0.059(8) 0.083(9) 0.220(18) -0.051(11) 0.003(10) 0.003(7)
C20 0.041(6) 0.065(7) 0.100(9) 0.002(6) 0.011(6) 0.012(5)
C21 0.069(4) 0.085(4) 0.149(5) -0.032(4) 0.014(4) -0.025(4)
C22 0.075(4) 0.095(4) 0.147(5) -0.026(4) 0.008(4) -0.030(4)
C23 0.060(4) 0.084(4) 0.122(5) -0.024(4) 0.015(4) -0.023(4)
C24 0.064(8) 0.160(14) 0.076(8) 0.023(8) -0.026(7) -0.026(8)
F1 0.161(12) 0.34(2) 0.192(12) 0.007(12) -0.049(9) -0.110(13)
F2 0.25(2) 0.30(2) 0.34(3) -0.164(19) 0.037(16) 0.085(17)
F3 0.56(4) 0.217(17) 0.256(19) -0.064(14) 0.12(2) -0.24(2)
F4 0.101(9) 0.54(3) 0.42(3) -0.27(3) -0.076(13) -0.012(15)
F5 0.32(2) 0.243(17) 0.37(2) -0.094(17) 0.061(18) 0.164(16)
F6 0.63(4) 0.231(18) 0.142(12) 0.037(12) -0.096(17) -0.13(2)
N1 0.038(5) 0.091(7) 0.058(5) -0.018(5) -0.005(4) 0.009(4)
N2 0.035(4) 0.069(5) 0.056(5) -0.001(4) 0.001(4) -0.006(4)
N3 0.038(4) 0.068(5) 0.042(4) -0.005(4) 0.004(4) -0.015(4)
N4 0.055(4) 0.077(4) 0.118(5) -0.027(4) 0.016(4) -0.022(4)
O1 0.045(4) 0.136(7) 0.078(5) 0.054(5) -0.009(4) -0.013(4)
O2 0.046(4) 0.074(5) 0.140(7) -0.013(5) 0.014(5) -0.004(4)
Os1 0.0357(2) 0.0629(2) 0.0444(2) 0.00208(19) 0.00470(17) -0.00348(18)
P1 0.076(3) 0.108(3) 0.158(5) -0.046(3) -0.019(3) -0.006(2)
S1 0.089(3) 0.094(2) 0.181(4) -0.035(3) 0.010(2) -0.033(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
C1 O1 1.338(13) . ?
C1 C6 1.377(19) . ?
C1 C2 1.399(19) . ?
C2 C3 1.33(2) . ?
C2 H2A 0.9300 . ?
C3 C4 1.35(3) . ?
C3 H3A 0.9300 . ?
C4 C5 1.42(3) . ?
C4 H4A 0.9300 . ?
C5 C6 1.421(17) . ?
C5 H5A 0.9300 . ?
C6 C7 1.445(17) . ?
C7 N1 1.304(13) . ?
C7 H7A 0.9300 . ?
C8 N1 1.448(13) . ?
C8 C13 1.545(14) . ?
C8 C9 1.548(15) . ?
C8 H8A 0.9800 . ?
C9 C10 1.53(2) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.535(19) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.531(16) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.511(14) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 N2 1.504(12) . ?
C13 H13A 0.9800 . ?
C14 N2 1.284(12) . ?
C14 C15 1.431(14) . ?
C14 H14A 0.9300 . ?
C15 C20 1.394(14) . ?
C15 C16 1.402(15) . ?
C16 C17 1.349(16) . ?
C16 H16A 0.9300 . ?
C17 C18 1.402(18) . ?
C17 H17A 0.9300 . ?
C18 C19 1.350(17) . ?
C18 H18A 0.9300 . ?
C19 C20 1.386(15) . ?
C19 H19A 0.9300 . ?
C20 O2 1.331(12) . ?
C21 N4 1.320(15) . ?
C21 S1 1.676(12) . ?
C21 H21A 0.9300 . ?
C22 C23 1.378(15) . ?
C22 S1 1.678(15) . ?
C22 H22A 0.9300 . ?
C23 N4 1.383(16) . ?
C23 C24 1.486(17) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
F1 P1 1.494(11) . ?
F2 P1 1.507(14) . ?
F3 P1 1.484(18) . ?
F4 P1 1.451(12) . ?
F5 P1 1.451(12) . ?
F6 P1 1.438(16) . ?
N1 Os1 2.023(8) . ?
N2 Os1 2.025(7) . ?
N3 N3 1.147(13) 5_556 ?
N3 Os1 1.869(7) . ?
N4 Os1 2.111(9) . ?
O1 Os1 1.963(7) . ?
O2 Os1 1.993(7) . ?
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
O1 C1 C6 123.2(13) . . ?
O1 C1 C2 116.9(15) . . ?
C6 C1 C2 119.9(13) . . ?
C3 C2 C1 121(2) . . ?
C3 C2 H2A 119.6 . . ?
C1 C2 H2A 119.6 . . ?
C2 C3 C4 121(2) . . ?
C2 C3 H3A 119.5 . . ?
C4 C3 H3A 119.5 . . ?
C3 C4 C5 121.5(18) . . ?
C3 C4 H4A 119.2 . . ?
C5 C4 H4A 119.2 . . ?
C4 C5 C6 116.7(18) . . ?
C4 C5 H5A 121.6 . . ?
C6 C5 H5A 121.6 . . ?
C1 C6 C5 119.8(16) . . ?
C1 C6 C7 118.9(11) . . ?
C5 C6 C7 120.5(17) . . ?
N1 C7 C6 125.3(11) . . ?
N1 C7 H7A 117.3 . . ?
C6 C7 H7A 117.3 . . ?
N1 C8 C13 105.6(9) . . ?
N1 C8 C9 117.9(10) . . ?
C13 C8 C9 109.3(9) . . ?
N1 C8 H8A 107.9 . . ?
C13 C8 H8A 107.9 . . ?
C9 C8 H8A 107.9 . . ?
C10 C9 C8 108.1(12) . . ?
C10 C9 H9A 110.1 . . ?
C8 C9 H9A 110.1 . . ?
C10 C9 H9B 110.1 . . ?
C8 C9 H9B 110.1 . . ?
H9A C9 H9B 108.4 . . ?
C9 C10 C11 110.4(14) . . ?
C9 C10 H10A 109.6 . . ?
C11 C10 H10A 109.6 . . ?
C9 C10 H10B 109.6 . . ?
C11 C10 H10B 109.6 . . ?
H10A C10 H10B 108.1 . . ?
C12 C11 C10 111.6(11) . . ?
C12 C11 H11A 109.3 . . ?
C10 C11 H11A 109.3 . . ?
C12 C11 H11B 109.3 . . ?
C10 C11 H11B 109.3 . . ?
H11A C11 H11B 108.0 . . ?
C13 C12 C11 110.1(10) . . ?
C13 C12 H12A 109.6 . . ?
C11 C12 H12A 109.6 . . ?
C13 C12 H12B 109.6 . . ?
C11 C12 H12B 109.6 . . ?
H12A C12 H12B 108.1 . . ?
N2 C13 C12 115.0(9) . . ?
N2 C13 C8 105.9(7) . . ?
C12 C13 C8 110.8(9) . . ?
N2 C13 H13A 108.3 . . ?
C12 C13 H13A 108.3 . . ?
C8 C13 H13A 108.3 . . ?
N2 C14 C15 126.2(9) . . ?
N2 C14 H14A 116.9 . . ?
C15 C14 H14A 116.9 . . ?
C20 C15 C16 118.1(10) . . ?
C20 C15 C14 125.0(10) . . ?
C16 C15 C14 116.8(10) . . ?
C17 C16 C15 123.7(12) . . ?
C17 C16 H16A 118.1 . . ?
C15 C16 H16A 118.1 . . ?
C16 C17 C18 117.1(12) . . ?
C16 C17 H17A 121.5 . . ?
C18 C17 H17A 121.5 . . ?
C19 C18 C17 120.5(13) . . ?
C19 C18 H18A 119.8 . . ?
C17 C18 H18A 119.8 . . ?
C18 C19 C20 122.8(13) . . ?
C18 C19 H19A 118.6 . . ?
C20 C19 H19A 118.6 . . ?
O2 C20 C19 115.8(11) . . ?
O2 C20 C15 126.5(9) . . ?
C19 C20 C15 117.7(10) . . ?
N4 C21 S1 115.0(11) . . ?
N4 C21 H21A 122.5 . . ?
S1 C21 H21A 122.5 . . ?
C23 C22 S1 111.8(11) . . ?
C23 C22 H22A 124.1 . . ?
S1 C22 H22A 124.1 . . ?
N4 C23 C22 112.0(13) . . ?
N4 C23 C24 122.2(10) . . ?
C22 C23 C24 125.8(13) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C7 N1 C8 124.7(10) . . ?
C7 N1 Os1 122.2(9) . . ?
C8 N1 Os1 109.4(6) . . ?
C14 N2 C13 120.7(8) . . ?
C14 N2 Os1 124.8(7) . . ?
C13 N2 Os1 114.5(6) . . ?
N3 N3 Os1 172.2(10) 5_556 . ?
C21 N4 C23 111.1(10) . . ?
C21 N4 Os1 118.4(9) . . ?
C23 N4 Os1 130.5(8) . . ?
C1 O1 Os1 119.9(7) . . ?
C20 O2 Os1 124.0(7) . . ?
N3 Os1 O1 174.6(3) . . ?
N3 Os1 O2 91.0(4) . . ?
O1 Os1 O2 86.8(4) . . ?
N3 Os1 N1 97.3(4) . . ?
O1 Os1 N1 85.5(4) . . ?
O2 Os1 N1 169.1(3) . . ?
N3 Os1 N2 91.3(3) . . ?
O1 Os1 N2 93.7(3) . . ?
O2 Os1 N2 92.9(3) . . ?
N1 Os1 N2 80.0(3) . . ?
N3 Os1 N4 90.5(4) . . ?
O1 Os1 N4 84.3(4) . . ?
O2 Os1 N4 85.3(3) . . ?
N1 Os1 N4 101.6(4) . . ?
N2 Os1 N4 177.4(4) . . ?
F6 P1 F5 89.8(12) . . ?
F6 P1 F4 89.3(13) . . ?
F5 P1 F4 87.3(11) . . ?
F6 P1 F3 176.5(11) . . ?
F5 P1 F3 91.2(12) . . ?
F4 P1 F3 94.1(13) . . ?
F6 P1 F1 86.2(10) . . ?
F5 P1 F1 100.1(11) . . ?
F4 P1 F1 171.3(13) . . ?
F3 P1 F1 90.3(10) . . ?
F6 P1 F2 93.4(13) . . ?
F5 P1 F2 176.8(14) . . ?
F4 P1 F2 93.2(11) . . ?
F3 P1 F2 85.6(11) . . ?
F1 P1 F2 79.7(10) . . ?
C21 S1 C22 90.1(7) . . ?
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full 24.99
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max 1.027
_refine_diff_density_min -0.889
_refine_diff_density_rms 0.126