# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2018
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
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# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
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data_jy105
_database_code_depnum_ccdc_archive 'CCDC 1859533'
_audit_update_record
;
2018-08-01 deposited with the CCDC.
2018-09-04 downloaded from the CCDC.
;
_audit_creation_method SHELXL-2014/7
_shelx_SHELXL_version_number 2014/7
_chemical_name_systematic
Chlorido-(1-methyl-4-isopropyl-benzene)-(N-n-butyl-(phenyl)(methylester)benzimidazol-\kN,C)osmium(II)
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C29 H33 Cl N2 O2 Os'
_chemical_formula_sum 'C29 H33 Cl N2 O2 Os'
_chemical_formula_weight 667.22
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'
Cl Cl 0.1484 0.1585 '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'
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 21/n'
_space_group_name_Hall '-P 2yn'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_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 11.0472(6)
_cell_length_b 19.7668(10)
_cell_length_c 12.2934(6)
_cell_angle_alpha 90
_cell_angle_beta 113.1612(18)
_cell_angle_gamma 90
_cell_volume 2468.1(2)
_cell_formula_units_Z 4
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 9768
_cell_measurement_theta_min 2.73
_cell_measurement_theta_max 30.49
_exptl_crystal_description prisms
_exptl_crystal_colour yellow
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_density_diffrn 1.796
_exptl_crystal_F_000 1320
_exptl_transmission_factor_min ?
_exptl_transmission_factor_max ?
_exptl_crystal_size_max 0.095
_exptl_crystal_size_mid 0.091
_exptl_crystal_size_min 0.076
_exptl_absorpt_coefficient_mu 5.305
_shelx_estimated_absorpt_T_min 0.633
_shelx_estimated_absorpt_T_max 0.689
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.6476
_exptl_absorpt_correction_T_max 0.7461
_exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)'
_exptl_absorpt_special_details ?
_diffrn_ambient_temperature 100(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 D8 QUEST CCD'
_diffrn_measurement_method '\w and \f scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 103770
_diffrn_reflns_av_unetI/netI 0.0418
_diffrn_reflns_av_R_equivalents 0.0767
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_k_min -28
_diffrn_reflns_limit_k_max 28
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_theta_min 2.061
_diffrn_reflns_theta_max 30.598
_diffrn_reflns_theta_full 25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total 7582
_reflns_number_gt 6178
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_max .
_reflns_Friedel_fraction_full .
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_computing_data_collection 'Bruker SMART'
_computing_cell_refinement 'Bruker SAINT'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'DIAMOND (Crystal Impact, 2017)'
_computing_publication_material 'SHELXL-97 (Sheldrick, 2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
Hydrogen atoms for aromatic CH, aliphatic CH, CH~2~ and methyl
groups were positioned geometrically (C---H = 0.95 \%A for aromatic CH, C---H
= 1.00 \%A for aliphatic CH, C---H = 0.99 \%A for CH~2~, C---H = 0.98 \%A for
CH~3~) and refined using a riding model (AFIX 43 for aromatic CH,
AFIX 13 for CH, AFIX 23 for CH~2~, AFIX 137 for rotating group for CH~3~),
with U~iso~(H) = 1.2U~eq~(CH,CH~2~) and U~iso~(H) = 1.5U~eq~(CH~3~).
The largest residual electron density peaks of 2.45 and 2.16 e \%A^-3^ are
within 1.0 \%A from
the Os atom, the deepest hole of -1.76 e \%A^-3^ is 0.77 \%A from the C5 atom.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+15.4911P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_number_reflns 7582
_refine_ls_number_parameters 321
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0608
_refine_ls_R_factor_gt 0.0407
_refine_ls_wR_factor_ref 0.0632
_refine_ls_wR_factor_gt 0.0588
_refine_ls_goodness_of_fit_ref 1.081
_refine_ls_restrained_S_all 1.081
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Os Os 0.06300(2) 0.21956(2) 0.84296(2) 0.00990(4) Uani 1 1 d . . . . .
Cl Cl -0.00637(9) 0.12136(5) 0.71638(8) 0.01456(18) Uani 1 1 d . . . . .
O1 O 0.5658(3) 0.06199(14) 1.0868(3) 0.0172(6) Uani 1 1 d . . . . .
O2 O 0.5660(3) -0.02374(15) 1.2082(3) 0.0174(6) Uani 1 1 d . . . . .
N1 N 0.0785(3) 0.14901(16) 0.9748(3) 0.0108(6) Uani 1 1 d . . . . .
N2 N -0.0094(3) 0.08400(16) 1.0739(3) 0.0102(6) Uani 1 1 d . . . . .
C1 C 0.1902(4) 0.2507(2) 0.7421(4) 0.0167(8) Uani 1 1 d . . . . .
C2 C 0.0726(4) 0.2896(2) 0.7088(3) 0.0164(8) Uani 1 1 d . . . . .
H2 H 0.0139 0.2918 0.6280 0.020 Uiso 1 1 calc R U . . .
C3 C 0.0423(4) 0.32504(19) 0.7954(4) 0.0155(8) Uani 1 1 d . . . . .
H3 H -0.0358 0.3514 0.7707 0.019 Uiso 1 1 calc R U . . .
C4 C 0.1253(4) 0.32237(19) 0.9179(3) 0.0149(8) Uani 1 1 d . . . . .
C5 C 0.2370(3) 0.2793(2) 0.9491(3) 0.0131(7) Uani 1 1 d . . . . .
H5 H 0.2897 0.2723 1.0306 0.016 Uiso 1 1 calc R U . . .
C6 C 0.2732(4) 0.2460(2) 0.8628(4) 0.0160(8) Uani 1 1 d . . . . .
H6 H 0.3426 0.2101 0.8892 0.019 Uiso 1 1 calc R U . . .
C7 C 0.2190(4) 0.2131(2) 0.6488(4) 0.0224(9) Uani 1 1 d . . . . .
H7A H 0.1502 0.1793 0.6118 0.034 Uiso 1 1 calc R U . . .
H7B H 0.3046 0.1905 0.6852 0.034 Uiso 1 1 calc R U . . .
H7C H 0.2212 0.2451 0.5887 0.034 Uiso 1 1 calc R U . . .
C8 C 0.1027(4) 0.3670(2) 1.0084(4) 0.0196(9) Uani 1 1 d . . . . .
H8 H 0.1585 0.3491 1.0886 0.024 Uiso 1 1 calc R U . . .
C9 C -0.0398(5) 0.3687(2) 0.9982(4) 0.0270(10) Uani 1 1 d . . . . .
H9A H -0.0958 0.3896 0.9229 0.041 Uiso 1 1 calc R U . . .
H9B H -0.0448 0.3952 1.0637 0.041 Uiso 1 1 calc R U . . .
H9C H -0.0702 0.3225 1.0015 0.041 Uiso 1 1 calc R U . . .
C10 C 0.1525(4) 0.4382(2) 0.9981(4) 0.0216(9) Uani 1 1 d . . . . .
H10A H 0.1015 0.4564 0.9191 0.032 Uiso 1 1 calc R U . . .
H10B H 0.2457 0.4359 1.0107 0.032 Uiso 1 1 calc R U . . .
H10C H 0.1422 0.4677 1.0579 0.032 Uiso 1 1 calc R U . . .
C11 C -0.0301(4) 0.13548(19) 0.9941(3) 0.0107(7) Uani 1 1 d . . . . .
C12 C 0.1192(4) 0.06226(19) 1.1047(3) 0.0110(7) Uani 1 1 d . . . . .
C13 C 0.1898(4) 0.00994(19) 1.1786(3) 0.0127(7) Uani 1 1 d . . . . .
H13 H 0.1527 -0.0171 1.2214 0.015 Uiso 1 1 calc R U . . .
C14 C 0.3166(4) -0.0005(2) 1.1862(3) 0.0136(8) Uani 1 1 d . . . . .
H14 H 0.3675 -0.0358 1.2353 0.016 Uiso 1 1 calc R U . . .
C15 C 0.3725(4) 0.03954(19) 1.1237(3) 0.0108(7) Uani 1 1 d . . . . .
C16 C 0.3019(4) 0.09230(18) 1.0504(3) 0.0098(7) Uani 1 1 d . . . . .
H16 H 0.3396 0.1197 1.0084 0.012 Uiso 1 1 calc R U . . .
C17 C 0.1739(4) 0.10299(18) 1.0417(3) 0.0104(7) Uani 1 1 d . . . . .
C18 C -0.0965(4) 0.0610(2) 1.1311(3) 0.0134(8) Uani 1 1 d . . . . .
H18A H -0.0629 0.0178 1.1729 0.016 Uiso 1 1 calc R U . . .
H18B H -0.1857 0.0527 1.0700 0.016 Uiso 1 1 calc R U . . .
C19 C -0.1044(4) 0.1139(2) 1.2197(4) 0.0173(8) Uani 1 1 d . . . . .
H19A H -0.1237 0.1585 1.1801 0.021 Uiso 1 1 calc R U . . .
H19B H -0.1790 0.1021 1.2417 0.021 Uiso 1 1 calc R U . . .
C20 C 0.0196(5) 0.1199(2) 1.3321(4) 0.0235(9) Uani 1 1 d . . . . .
H20A H 0.0970 0.1222 1.3105 0.028 Uiso 1 1 calc R U . . .
H20B H 0.0162 0.1627 1.3725 0.028 Uiso 1 1 calc R U . . .
C21 C 0.0377(5) 0.0616(3) 1.4170(4) 0.0326(11) Uani 1 1 d . . . . .
H21A H 0.0333 0.0187 1.3756 0.049 Uiso 1 1 calc R U . . .
H21B H -0.0321 0.0628 1.4473 0.049 Uiso 1 1 calc R U . . .
H21C H 0.1237 0.0655 1.4831 0.049 Uiso 1 1 calc R U . . .
C22 C 0.5106(4) 0.02817(19) 1.1350(3) 0.0122(7) Uani 1 1 d . . . . .
C23 C 0.7019(4) -0.0378(2) 1.2310(4) 0.0233(9) Uani 1 1 d . . . . .
H23A H 0.7138 -0.0381 1.1561 0.035 Uiso 1 1 calc R U . . .
H23B H 0.7263 -0.0820 1.2694 0.035 Uiso 1 1 calc R U . . .
H23C H 0.7580 -0.0027 1.2830 0.035 Uiso 1 1 calc R U . . .
C24 C -0.1486(4) 0.17188(19) 0.9220(3) 0.0120(7) Uani 1 1 d . . . . .
C25 C -0.2754(4) 0.1624(2) 0.9214(3) 0.0157(8) Uani 1 1 d . . . . .
H25 H -0.2880 0.1334 0.9777 0.019 Uiso 1 1 calc R U . . .
C26 C -0.3810(4) 0.1958(2) 0.8380(4) 0.0210(9) Uani 1 1 d . . . . .
H26 H -0.4671 0.1891 0.8357 0.025 Uiso 1 1 calc R U . . .
C27 C -0.3616(4) 0.2391(2) 0.7575(4) 0.0188(9) Uani 1 1 d . . . . .
H27 H -0.4347 0.2618 0.7002 0.023 Uiso 1 1 calc R U . . .
C28 C -0.2362(4) 0.2496(2) 0.7601(4) 0.0156(8) Uani 1 1 d . . . . .
H28 H -0.2252 0.2802 0.7052 0.019 Uiso 1 1 calc R U . . .
C29 C -0.1250(3) 0.2162(2) 0.8416(3) 0.0118(7) 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
Os 0.01036(6) 0.00764(6) 0.01014(6) 0.00243(6) 0.00234(5) 0.00017(6)
Cl 0.0164(4) 0.0119(4) 0.0157(4) -0.0018(3) 0.0066(4) -0.0018(3)
O1 0.0135(14) 0.0165(14) 0.0222(15) 0.0033(12) 0.0075(12) 0.0007(11)
O2 0.0123(13) 0.0178(15) 0.0211(15) 0.0062(12) 0.0053(12) 0.0036(11)
N1 0.0102(14) 0.0081(15) 0.0114(15) 0.0014(12) 0.0014(12) -0.0009(12)
N2 0.0081(14) 0.0098(15) 0.0116(15) 0.0013(12) 0.0028(12) 0.0013(12)
C1 0.019(2) 0.0159(19) 0.0168(19) 0.0036(16) 0.0081(16) -0.0060(16)
C2 0.0207(19) 0.013(2) 0.0132(18) 0.0070(15) 0.0043(15) -0.0023(16)
C3 0.019(2) 0.0071(18) 0.0148(19) 0.0000(14) 0.0003(16) -0.0014(15)
C4 0.019(2) 0.0098(18) 0.0148(19) 0.0039(15) 0.0059(16) -0.0012(15)
C5 0.0086(16) 0.0152(18) 0.0114(16) 0.0022(16) -0.0005(13) -0.0042(16)
C6 0.0145(19) 0.0140(19) 0.020(2) 0.0035(16) 0.0067(16) -0.0022(15)
C7 0.028(2) 0.022(2) 0.021(2) 0.0039(18) 0.0137(18) -0.0017(19)
C8 0.025(2) 0.014(2) 0.017(2) -0.0022(16) 0.0064(18) -0.0018(17)
C9 0.028(2) 0.024(2) 0.031(3) -0.009(2) 0.014(2) -0.0010(19)
C10 0.026(2) 0.014(2) 0.020(2) -0.0041(17) 0.0035(18) -0.0033(17)
C11 0.0118(17) 0.0093(17) 0.0094(17) -0.0004(14) 0.0026(14) -0.0001(14)
C12 0.0116(17) 0.0099(17) 0.0122(17) -0.0014(14) 0.0052(14) -0.0008(14)
C13 0.0176(19) 0.0095(18) 0.0108(17) 0.0030(14) 0.0052(15) 0.0012(14)
C14 0.0129(18) 0.0130(18) 0.0115(18) 0.0012(15) 0.0010(15) 0.0006(15)
C15 0.0105(17) 0.0097(17) 0.0107(17) -0.0009(14) 0.0026(14) -0.0002(14)
C16 0.0113(17) 0.0079(17) 0.0107(17) -0.0019(13) 0.0048(14) -0.0028(13)
C17 0.0134(18) 0.0079(17) 0.0080(17) -0.0011(13) 0.0022(14) -0.0014(14)
C18 0.0091(17) 0.0172(19) 0.0145(19) 0.0038(15) 0.0052(14) -0.0012(14)
C19 0.018(2) 0.017(2) 0.020(2) 0.0020(16) 0.0103(17) 0.0019(16)
C20 0.026(2) 0.024(2) 0.019(2) -0.0044(18) 0.0079(19) -0.0015(18)
C21 0.043(3) 0.027(3) 0.020(2) 0.002(2) 0.004(2) 0.000(2)
C22 0.0113(18) 0.0108(18) 0.0119(18) -0.0035(14) 0.0019(15) 0.0000(14)
C23 0.0127(19) 0.027(2) 0.028(2) 0.0109(19) 0.0059(18) 0.0085(17)
C24 0.0108(17) 0.0113(18) 0.0127(18) -0.0024(14) 0.0031(14) 0.0026(14)
C25 0.0133(18) 0.018(2) 0.0162(19) -0.0008(16) 0.0066(15) 0.0007(15)
C26 0.0118(19) 0.028(2) 0.022(2) -0.0024(18) 0.0054(17) 0.0043(17)
C27 0.0123(18) 0.023(2) 0.018(2) -0.0005(16) 0.0022(16) 0.0100(16)
C28 0.0160(19) 0.0146(19) 0.0150(19) 0.0026(16) 0.0049(16) 0.0043(15)
C29 0.0121(16) 0.0108(17) 0.0119(16) -0.0024(15) 0.0041(13) 0.0019(15)
_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
Os C29 2.071(4) . ?
Os N1 2.093(3) . ?
Os C3 2.153(4) . ?
Os C2 2.187(4) . ?
Os C5 2.195(4) . ?
Os C4 2.226(4) . ?
Os C1 2.294(4) . ?
Os C6 2.298(4) . ?
Os Cl 2.4164(9) . ?
O1 C22 1.206(5) . ?
O2 C22 1.343(5) . ?
O2 C23 1.442(5) . ?
N1 C11 1.339(5) . ?
N1 C17 1.390(5) . ?
N2 C11 1.368(5) . ?
N2 C12 1.387(5) . ?
N2 C18 1.470(5) . ?
C1 C6 1.408(6) . ?
C1 C2 1.424(6) . ?
C1 C7 1.501(6) . ?
C2 C3 1.419(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.423(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.422(5) . ?
C4 C8 1.515(6) . ?
C5 C6 1.433(6) . ?
C5 H5 0.9500 . ?
C6 H6 1.0000 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.530(6) . ?
C8 C10 1.535(6) . ?
C8 H8 1.0000 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C24 1.451(5) . ?
C12 C13 1.394(5) . ?
C12 C17 1.408(5) . ?
C13 C14 1.382(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.404(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.398(5) . ?
C15 C22 1.493(5) . ?
C16 C17 1.391(5) . ?
C16 H16 0.9500 . ?
C18 C19 1.537(6) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.521(6) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.515(6) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.410(5) . ?
C24 C29 1.420(5) . ?
C25 C26 1.381(6) . ?
C25 H25 0.9500 . ?
C26 C27 1.387(6) . ?
C26 H26 0.9500 . ?
C27 C28 1.389(6) . ?
C27 H27 0.9500 . ?
C28 C29 1.407(5) . ?
C28 H28 0.9500 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C29 Os N1 76.22(14) . . ?
C29 Os C3 91.70(16) . . ?
N1 Os C3 145.40(14) . . ?
C29 Os C2 111.08(15) . . ?
N1 Os C2 172.64(14) . . ?
C3 Os C2 38.16(15) . . ?
C29 Os C5 131.50(14) . . ?
N1 Os C5 96.44(13) . . ?
C3 Os C5 67.37(15) . . ?
C2 Os C5 79.46(14) . . ?
C29 Os C4 100.28(15) . . ?
N1 Os C4 111.74(13) . . ?
C3 Os C4 37.88(15) . . ?
C2 Os C4 68.60(15) . . ?
C5 Os C4 37.51(15) . . ?
C29 Os C1 146.05(15) . . ?
N1 Os C1 135.74(14) . . ?
C3 Os C1 67.38(16) . . ?
C2 Os C1 36.96(15) . . ?
C5 Os C1 66.29(14) . . ?
C4 Os C1 79.81(15) . . ?
C29 Os C6 167.52(15) . . ?
N1 Os C6 107.31(13) . . ?
C3 Os C6 78.67(15) . . ?
C2 Os C6 65.77(15) . . ?
C5 Os C6 37.11(14) . . ?
C4 Os C6 67.24(15) . . ?
C1 Os C6 35.71(14) . . ?
C29 Os Cl 84.62(11) . . ?
N1 Os Cl 82.64(9) . . ?
C3 Os Cl 129.05(11) . . ?
C2 Os Cl 96.89(11) . . ?
C5 Os Cl 142.81(11) . . ?
C4 Os Cl 165.49(10) . . ?
C1 Os Cl 88.50(11) . . ?
C6 Os Cl 107.59(11) . . ?
C22 O2 C23 116.3(3) . . ?
C11 N1 C17 106.7(3) . . ?
C11 N1 Os 117.7(2) . . ?
C17 N1 Os 135.0(3) . . ?
C11 N2 C12 106.9(3) . . ?
C11 N2 C18 128.1(3) . . ?
C12 N2 C18 124.5(3) . . ?
C6 C1 C2 118.7(4) . . ?
C6 C1 C7 121.7(4) . . ?
C2 C1 C7 119.4(4) . . ?
C6 C1 Os 72.3(2) . . ?
C2 C1 Os 67.5(2) . . ?
C7 C1 Os 129.7(3) . . ?
C3 C2 C1 120.6(4) . . ?
C3 C2 Os 69.6(2) . . ?
C1 C2 Os 75.6(2) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
Os C2 H2 127.0 . . ?
C2 C3 C4 122.1(4) . . ?
C2 C3 Os 72.2(2) . . ?
C4 C3 Os 73.8(2) . . ?
C2 C3 H3 119.0 . . ?
C4 C3 H3 119.0 . . ?
Os C3 H3 127.1 . . ?
C5 C4 C3 116.0(4) . . ?
C5 C4 C8 121.7(4) . . ?
C3 C4 C8 122.1(4) . . ?
C5 C4 Os 70.1(2) . . ?
C3 C4 Os 68.3(2) . . ?
C8 C4 Os 136.2(3) . . ?
C4 C5 C6 122.7(3) . . ?
C4 C5 Os 72.4(2) . . ?
C6 C5 Os 75.3(2) . . ?
C4 C5 H5 118.6 . . ?
C6 C5 H5 118.6 . . ?
Os C5 H5 125.4 . . ?
C1 C6 C5 119.6(4) . . ?
C1 C6 Os 72.0(2) . . ?
C5 C6 Os 67.5(2) . . ?
C1 C6 H6 119.2 . . ?
C5 C6 H6 119.2 . . ?
Os C6 H6 119.2 . . ?
C1 C7 H7A 109.5 . . ?
C1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C4 C8 C9 114.5(4) . . ?
C4 C8 C10 107.8(3) . . ?
C9 C8 C10 111.3(4) . . ?
C4 C8 H8 107.7 . . ?
C9 C8 H8 107.7 . . ?
C10 C8 H8 107.7 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 N2 111.5(3) . . ?
N1 C11 C24 116.6(3) . . ?
N2 C11 C24 131.5(3) . . ?
N2 C12 C13 131.2(3) . . ?
N2 C12 C17 106.7(3) . . ?
C13 C12 C17 122.1(3) . . ?
C14 C13 C12 116.5(3) . . ?
C14 C13 H13 121.7 . . ?
C12 C13 H13 121.7 . . ?
C13 C14 C15 122.1(4) . . ?
C13 C14 H14 118.9 . . ?
C15 C14 H14 118.9 . . ?
C16 C15 C14 121.2(3) . . ?
C16 C15 C22 117.6(3) . . ?
C14 C15 C22 121.2(3) . . ?
C17 C16 C15 117.1(3) . . ?
C17 C16 H16 121.4 . . ?
C15 C16 H16 121.4 . . ?
N1 C17 C16 131.0(3) . . ?
N1 C17 C12 108.1(3) . . ?
C16 C17 C12 120.9(3) . . ?
N2 C18 C19 111.0(3) . . ?
N2 C18 H18A 109.4 . . ?
C19 C18 H18A 109.4 . . ?
N2 C18 H18B 109.4 . . ?
C19 C18 H18B 109.4 . . ?
H18A C18 H18B 108.0 . . ?
C20 C19 C18 114.5(3) . . ?
C20 C19 H19A 108.6 . . ?
C18 C19 H19A 108.6 . . ?
C20 C19 H19B 108.6 . . ?
C18 C19 H19B 108.6 . . ?
H19A C19 H19B 107.6 . . ?
C21 C20 C19 113.2(4) . . ?
C21 C20 H20A 108.9 . . ?
C19 C20 H20A 108.9 . . ?
C21 C20 H20B 108.9 . . ?
C19 C20 H20B 108.9 . . ?
H20A C20 H20B 107.8 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O1 C22 O2 124.6(4) . . ?
O1 C22 C15 124.5(4) . . ?
O2 C22 C15 110.9(3) . . ?
O2 C23 H23A 109.5 . . ?
O2 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
O2 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 C29 122.2(3) . . ?
C25 C24 C11 126.4(4) . . ?
C29 C24 C11 111.3(3) . . ?
C26 C25 C24 119.2(4) . . ?
C26 C25 H25 120.4 . . ?
C24 C25 H25 120.4 . . ?
C25 C26 C27 120.1(4) . . ?
C25 C26 H26 119.9 . . ?
C27 C26 H26 119.9 . . ?
C26 C27 C28 120.5(4) . . ?
C26 C27 H27 119.7 . . ?
C28 C27 H27 119.7 . . ?
C27 C28 C29 122.1(4) . . ?
C27 C28 H28 119.0 . . ?
C29 C28 H28 119.0 . . ?
C28 C29 C24 115.9(3) . . ?
C28 C29 Os 125.7(3) . . ?
C24 C29 Os 118.2(3) . . ?
_refine_diff_density_max 2.451
_refine_diff_density_min -1.757
_refine_diff_density_rms 0.201
_shelx_res_file
;
jy105.res created by SHELXL-2014/7
TITL jy105 in P2(1)/n
CELL 0.71073 11.04720 19.76680 12.29340 90.0000 113.1612 90.0000
ZERR 4.00 0.00060 0.00100 0.00060 0.0000 0.0018 0.0000
LATT 1
SYMM 0.5-X, 0.5+Y, 0.5-Z
SFAC C H N O CL OS
UNIT 116 132 8 8 4 4
LIST 4
TEMP -173.150
SIZE 0.076 0.091 0.095
L.S. 6
BOND $H
ACTA
FMAP 2
PLAN 20
WGHT 0.000000 15.491100
FVAR 0.08491
OS 6 0.062998 0.219562 0.842962 11.00000 0.01036 0.00764 =
0.01014 0.00243 0.00234 0.00017
CL 5 -0.006366 0.121356 0.716376 11.00000 0.01641 0.01192 =
0.01565 -0.00177 0.00662 -0.00182
O1 4 0.565768 0.061992 1.086795 11.00000 0.01351 0.01651 =
0.02221 0.00328 0.00755 0.00069
O2 4 0.565997 -0.023741 1.208235 11.00000 0.01226 0.01780 =
0.02105 0.00616 0.00530 0.00357
N1 3 0.078531 0.149007 0.974769 11.00000 0.01020 0.00810 =
0.01145 0.00139 0.00139 -0.00086
N2 3 -0.009412 0.083997 1.073890 11.00000 0.00812 0.00980 =
0.01160 0.00132 0.00283 0.00130
C1 1 0.190167 0.250685 0.742081 11.00000 0.01865 0.01590 =
0.01676 0.00356 0.00815 -0.00600
C2 1 0.072597 0.289590 0.708833 11.00000 0.02069 0.01300 =
0.01321 0.00699 0.00428 -0.00232
AFIX 43
H2 2 0.013912 0.291836 0.628025 11.00000 -1.20000
AFIX 0
C3 1 0.042325 0.325043 0.795371 11.00000 0.01882 0.00715 =
0.01481 0.00003 0.00034 -0.00137
AFIX 43
H3 2 -0.035822 0.351385 0.770744 11.00000 -1.20000
AFIX 0
C4 1 0.125340 0.322370 0.917852 11.00000 0.01945 0.00984 =
0.01478 0.00388 0.00592 -0.00116
C5 1 0.236980 0.279284 0.949119 11.00000 0.00857 0.01520 =
0.01140 0.00223 -0.00046 -0.00421
AFIX 43
H5 2 0.289729 0.272289 1.030579 11.00000 -1.20000
AFIX 0
C6 1 0.273213 0.245973 0.862815 11.00000 0.01453 0.01400 =
0.01960 0.00349 0.00670 -0.00223
AFIX 13
H6 2 0.342623 0.210112 0.889199 11.00000 -1.20000
AFIX 0
C7 1 0.219047 0.213127 0.648841 11.00000 0.02757 0.02225 =
0.02124 0.00386 0.01366 -0.00170
AFIX 137
H7A 2 0.150207 0.179304 0.611766 11.00000 -1.50000
H7B 2 0.304569 0.190496 0.685236 11.00000 -1.50000
H7C 2 0.221213 0.245068 0.588664 11.00000 -1.50000
AFIX 0
C8 1 0.102721 0.366960 1.008372 11.00000 0.02545 0.01399 =
0.01747 -0.00224 0.00639 -0.00182
AFIX 13
H8 2 0.158503 0.349089 1.088645 11.00000 -1.20000
AFIX 0
C9 1 -0.039807 0.368721 0.998197 11.00000 0.02842 0.02365 =
0.03126 -0.00933 0.01420 -0.00098
AFIX 137
H9A 2 -0.095780 0.389625 0.922856 11.00000 -1.50000
H9B 2 -0.044760 0.395190 1.063728 11.00000 -1.50000
H9C 2 -0.070170 0.322477 1.001490 11.00000 -1.50000
AFIX 0
C10 1 0.152530 0.438179 0.998080 11.00000 0.02619 0.01359 =
0.01982 -0.00415 0.00348 -0.00332
AFIX 137
H10A 2 0.101475 0.456383 0.919052 11.00000 -1.50000
H10B 2 0.245738 0.435911 1.010743 11.00000 -1.50000
H10C 2 0.142182 0.467719 1.057871 11.00000 -1.50000
AFIX 0
C11 1 -0.030118 0.135475 0.994146 11.00000 0.01175 0.00932 =
0.00942 -0.00041 0.00258 -0.00015
C12 1 0.119229 0.062259 1.104740 11.00000 0.01157 0.00986 =
0.01219 -0.00137 0.00521 -0.00080
C13 1 0.189800 0.009942 1.178585 11.00000 0.01762 0.00948 =
0.01077 0.00302 0.00523 0.00117
AFIX 43
H13 2 0.152652 -0.017140 1.221434 11.00000 -1.20000
AFIX 0
C14 1 0.316551 -0.000455 1.186188 11.00000 0.01289 0.01298 =
0.01154 0.00116 0.00104 0.00057
AFIX 43
H14 2 0.367494 -0.035819 1.235291 11.00000 -1.20000
AFIX 0
C15 1 0.372508 0.039544 1.123701 11.00000 0.01054 0.00973 =
0.01068 -0.00092 0.00263 -0.00015
C16 1 0.301853 0.092302 1.050440 11.00000 0.01127 0.00791 =
0.01075 -0.00186 0.00480 -0.00275
AFIX 43
H16 2 0.339594 0.119661 1.008423 11.00000 -1.20000
AFIX 0
C17 1 0.173930 0.102994 1.041739 11.00000 0.01339 0.00786 =
0.00800 -0.00108 0.00225 -0.00136
C18 1 -0.096511 0.060961 1.131075 11.00000 0.00908 0.01718 =
0.01449 0.00380 0.00523 -0.00116
AFIX 23
H18A 2 -0.062853 0.017803 1.172910 11.00000 -1.20000
H18B 2 -0.185747 0.052659 1.070015 11.00000 -1.20000
AFIX 0
C19 1 -0.104444 0.113873 1.219660 11.00000 0.01779 0.01717 =
0.01974 0.00201 0.01033 0.00185
AFIX 23
H19A 2 -0.123731 0.158530 1.180051 11.00000 -1.20000
H19B 2 -0.178974 0.102139 1.241664 11.00000 -1.20000
AFIX 0
C20 1 0.019648 0.119926 1.332067 11.00000 0.02646 0.02384 =
0.01910 -0.00436 0.00785 -0.00149
AFIX 23
H20A 2 0.096977 0.122154 1.310506 11.00000 -1.20000
H20B 2 0.016157 0.162729 1.372549 11.00000 -1.20000
AFIX 0
C21 1 0.037744 0.061588 1.417020 11.00000 0.04317 0.02733 =
0.01953 0.00225 0.00384 0.00013
AFIX 137
H21A 2 0.033326 0.018728 1.375558 11.00000 -1.50000
H21B 2 -0.032062 0.062801 1.447345 11.00000 -1.50000
H21C 2 0.123672 0.065508 1.483100 11.00000 -1.50000
AFIX 0
C22 1 0.510559 0.028171 1.135007 11.00000 0.01135 0.01076 =
0.01190 -0.00352 0.00187 -0.00001
C23 1 0.701905 -0.037786 1.230999 11.00000 0.01268 0.02690 =
0.02834 0.01087 0.00593 0.00852
AFIX 137
H23A 2 0.713813 -0.038136 1.156102 11.00000 -1.50000
H23B 2 0.726297 -0.082031 1.269411 11.00000 -1.50000
H23C 2 0.757974 -0.002737 1.282955 11.00000 -1.50000
AFIX 0
C24 1 -0.148605 0.171881 0.922004 11.00000 0.01076 0.01127 =
0.01268 -0.00242 0.00313 0.00264
C25 1 -0.275381 0.162428 0.921397 11.00000 0.01330 0.01831 =
0.01625 -0.00077 0.00664 0.00066
AFIX 43
H25 2 -0.287970 0.133445 0.977708 11.00000 -1.20000
AFIX 0
C26 1 -0.381013 0.195786 0.838003 11.00000 0.01176 0.02821 =
0.02180 -0.00236 0.00542 0.00426
AFIX 43
H26 2 -0.467123 0.189065 0.835737 11.00000 -1.20000
AFIX 0
C27 1 -0.361627 0.239097 0.757525 11.00000 0.01226 0.02295 =
0.01786 -0.00051 0.00224 0.00997
AFIX 43
H27 2 -0.434736 0.261775 0.700164 11.00000 -1.20000
AFIX 0
C28 1 -0.236202 0.249572 0.760132 11.00000 0.01602 0.01461 =
0.01501 0.00264 0.00491 0.00428
AFIX 43
H28 2 -0.225178 0.280207 0.705187 11.00000 -1.20000
AFIX 0
C29 1 -0.124980 0.216238 0.841586 11.00000 0.01214 0.01077 =
0.01186 -0.00235 0.00407 0.00188
HKLF 4
REM jy105 in P2(1)/n
REM R1 = 0.0407 for 6178 Fo > 4sig(Fo) and 0.0608 for all 7582 data
REM 321 parameters refined using 0 restraints
END
WGHT 0.0000 15.4912
REM Highest difference peak 2.451, deepest hole -1.757, 1-sigma level 0.201
Q1 1 0.1490 0.2086 0.8824 11.00000 0.05 2.45
Q2 1 0.0261 0.2312 0.8787 11.00000 0.05 2.16
Q3 1 0.3173 0.2692 0.9190 11.00000 0.05 0.87
Q4 1 0.1180 0.3053 1.1596 11.00000 0.05 0.79
Q5 1 0.2613 0.2508 0.7822 11.00000 0.05 0.79
Q6 1 -0.2552 0.1621 0.9831 11.00000 0.05 0.78
Q7 1 -0.1803 0.0654 1.2817 11.00000 0.05 0.78
Q8 1 -0.0157 0.2248 0.7807 11.00000 0.05 0.78
Q9 1 0.0569 0.1954 0.7578 11.00000 0.05 0.77
Q10 1 -0.0737 0.0101 1.4425 11.00000 0.05 0.76
Q11 1 0.2359 0.2389 1.0693 11.00000 0.05 0.75
Q12 1 0.0521 0.1050 1.4671 11.00000 0.05 0.73
Q13 1 0.0476 0.1998 0.6766 11.00000 0.05 0.73
Q14 1 0.1588 -0.0570 1.2379 11.00000 0.05 0.72
Q15 1 -0.1322 0.1044 1.3339 11.00000 0.05 0.72
Q16 1 -0.0987 0.2171 0.7251 11.00000 0.05 0.72
Q17 1 0.2664 0.1195 1.0831 11.00000 0.05 0.72
Q18 1 0.2961 0.2716 1.0942 11.00000 0.05 0.71
Q19 1 0.2989 0.2488 0.9755 11.00000 0.05 0.71
Q20 1 0.0082 0.0736 1.3396 11.00000 0.05 0.71
;
_shelx_res_checksum 50552
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methylene chloride, hexane, toluene'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_jY85
_database_code_depnum_ccdc_archive 'CCDC 1859534'
_audit_update_record
;
2018-08-01 deposited with the CCDC.
2018-09-04 downloaded from the CCDC.
;
_audit_creation_method SHELXL-2014/7
_shelx_SHELXL_version_number 2014/7
_chemical_name_systematic
'Acetato-(1-methyl-4-isopropyl-benzene)-(N-n-butyl-(4-biphenyl)(methylester)benzimidazol-\kN,C)osmium(II)hemi-dichloromethane, hemi-toluene solvate'
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C37 H40 N2 O4 Os, 0.5(C7 H8), 0.5(C H2 Cl2)'
_chemical_formula_sum 'C41 H45 Cl N2 O4 Os'
_chemical_formula_weight 855.44
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'
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'
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 10.9559(6)
_cell_length_b 10.9932(6)
_cell_length_c 16.2594(9)
_cell_angle_alpha 105.966(2)
_cell_angle_beta 102.536(2)
_cell_angle_gamma 103.578(2)
_cell_volume 1745.05(17)
_cell_formula_units_Z 2
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 9621
_cell_measurement_theta_min 2.68
_cell_measurement_theta_max 28.37
_exptl_crystal_description block
_exptl_crystal_colour orange
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_density_diffrn 1.628
_exptl_crystal_F_000 860
_exptl_transmission_factor_min ?
_exptl_transmission_factor_max ?
_exptl_crystal_size_max 0.213
_exptl_crystal_size_mid 0.131
_exptl_crystal_size_min 0.126
_exptl_absorpt_coefficient_mu 3.776
_shelx_estimated_absorpt_T_min 0.500
_shelx_estimated_absorpt_T_max 0.648
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.6233
_exptl_absorpt_correction_T_max 0.7457
_exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)'
_exptl_absorpt_special_details ?
_diffrn_ambient_temperature 100(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 D8 QUEST CCD'
_diffrn_measurement_method '\w and \f scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 85900
_diffrn_reflns_av_unetI/netI 0.0269
_diffrn_reflns_av_R_equivalents 0.0470
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_theta_min 2.005
_diffrn_reflns_theta_max 28.389
_diffrn_reflns_theta_full 25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total 8746
_reflns_number_gt 7910
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_max .
_reflns_Friedel_fraction_full .
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_computing_data_collection 'Bruker SMART'
_computing_cell_refinement 'Bruker SAINT'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'DIAMOND (Crystal Impact, 2017)'
_computing_publication_material 'SHELXL-97 (Sheldrick, 2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
Hydrogen atoms for aromatic CH, aliphatic CH, CH~2~ and methyl
groups were positioned geometrically (C---H = 0.95 \%A for aromatic CH, C---H
= 1.00 \%A for aliphatic CH, C---H = 0.99 \%A for CH~2~, C---H = 0.98 \%A for
CH~3~) and refined using a riding model (AFIX 43 for aromatic CH,
AFIX 13 for CH, AFIX 23 for CH~2~, AFIX 137 for rotating group for CH~3~),
with U~iso~(H) = 1.2U~eq~(CH,CH~2~) and U~iso~(H) = 1.5U~eq~(CH~3~).
The dichloromethane and toluene crystal solvent molecules share a common
position. They were both refined to half-occupancy with PART commands. For
toluene the PART -n command was used as the toluene molecule sits
around the inversion center.
The phenyl ring of the toluene molecule was refined as a rigid group
using AFIX 66 1.39 to fits the following next six non-H atoms to a
regular hexagon with C-C = 1.39 \%A.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0112P)^2^+3.9323P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_number_reflns 8746
_refine_ls_number_parameters 482
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0333
_refine_ls_R_factor_gt 0.0267
_refine_ls_wR_factor_ref 0.0530
_refine_ls_wR_factor_gt 0.0511
_refine_ls_goodness_of_fit_ref 1.119
_refine_ls_restrained_S_all 1.119
_refine_ls_shift/su_max 0.005
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Os Os 0.12021(2) 1.02450(2) 0.27458(2) 0.01486(4) Uani 1 1 d . . . . .
O1 O -0.2086(2) 0.3498(2) -0.05366(14) 0.0330(5) Uani 1 1 d . . . . .
O2 O -0.1679(2) 0.5603(2) -0.05095(13) 0.0295(5) Uani 1 1 d . . . . .
O3 O -0.0711(2) 1.0321(2) 0.26813(13) 0.0206(4) Uani 1 1 d . . . . .
O4 O -0.0274(2) 1.2520(2) 0.33910(15) 0.0275(5) Uani 1 1 d . . . . .
N5 N 0.0415(2) 0.8389(2) 0.28461(14) 0.0143(4) Uani 1 1 d . . . . .
N8 N 0.0142(2) 0.7007(2) 0.36188(15) 0.0140(4) Uani 1 1 d . . . . .
C1 C 0.1157(3) 1.1218(3) 0.16988(19) 0.0229(6) Uani 1 1 d . . . . .
C2 C 0.2132(3) 1.2074(3) 0.25287(19) 0.0211(6) Uani 1 1 d . . . . .
H2 H 0.2130 1.2959 0.2794 0.025 Uiso 1 1 calc R U . . .
C3 C 0.3096(3) 1.1603(3) 0.29546(19) 0.0203(6) Uani 1 1 d . . . . .
H3 H 0.3733 1.2187 0.3505 0.024 Uiso 1 1 calc R U . . .
C4 C 0.3153(3) 1.0284(3) 0.25893(19) 0.0206(6) Uani 1 1 d . . . . .
C5 C 0.2150(3) 0.9452(3) 0.17783(19) 0.0204(6) Uani 1 1 d . . . . .
H5 H 0.2108 0.8546 0.1538 0.025 Uiso 1 1 calc R U . . .
C6 C 0.1203(3) 0.9913(3) 0.13079(19) 0.0230(6) Uani 1 1 d . . . . .
H6 H 0.0607 0.9349 0.0737 0.028 Uiso 1 1 calc R U . . .
C7 C 0.0073(3) 1.1668(3) 0.1279(2) 0.0283(7) Uani 1 1 d . . . . .
H7A H 0.0317 1.2036 0.0832 0.042 Uiso 1 1 calc R U . . .
H7B H -0.0073 1.2354 0.1743 0.042 Uiso 1 1 calc R U . . .
H7C H -0.0736 1.0908 0.0987 0.042 Uiso 1 1 calc R U . . .
C8 C 0.4202(3) 0.9779(3) 0.3030(2) 0.0257(7) Uani 1 1 d . . . . .
H8 H 0.4824 0.9732 0.2662 0.031 Uiso 1 1 calc R U . . .
C9 C 0.3640(4) 0.8373(3) 0.3045(3) 0.0393(9) Uani 1 1 d . . . . .
H9A H 0.4364 0.8054 0.3270 0.059 Uiso 1 1 calc R U . . .
H9B H 0.3119 0.7772 0.2437 0.059 Uiso 1 1 calc R U . . .
H9C H 0.3078 0.8394 0.3439 0.059 Uiso 1 1 calc R U . . .
C10 C 0.5009(3) 1.0693(3) 0.3977(2) 0.0328(7) Uani 1 1 d . . . . .
H10A H 0.5667 1.0313 0.4222 0.049 Uiso 1 1 calc R U . . .
H10B H 0.4426 1.0786 0.4355 0.049 Uiso 1 1 calc R U . . .
H10C H 0.5455 1.1570 0.3967 0.049 Uiso 1 1 calc R U . . .
C11 C 0.0606(3) 0.8304(3) 0.36666(17) 0.0135(5) Uani 1 1 d . . . . .
C12 C -0.0381(3) 0.6236(3) 0.27221(17) 0.0149(5) Uani 1 1 d . . . . .
C13 C -0.0964(3) 0.4860(3) 0.22911(19) 0.0185(6) Uani 1 1 d . . . . .
H13 H -0.1065 0.4271 0.2621 0.022 Uiso 1 1 calc R U . . .
C14 C -0.1387(3) 0.4396(3) 0.13634(19) 0.0203(6) Uani 1 1 d . . . . .
H14 H -0.1795 0.3468 0.1048 0.024 Uiso 1 1 calc R U . . .
C15 C -0.1227(3) 0.5270(3) 0.08757(19) 0.0201(6) Uani 1 1 d . . . . .
C16 C -0.0635(3) 0.6636(3) 0.13061(18) 0.0182(6) Uani 1 1 d . . . . .
H16 H -0.0524 0.7224 0.0976 0.022 Uiso 1 1 calc R U . . .
C17 C -0.0214(3) 0.7108(3) 0.22378(17) 0.0151(5) Uani 1 1 d . . . . .
C18 C 0.0355(3) 0.6465(3) 0.43526(18) 0.0162(5) Uani 1 1 d . . . . .
H18A H -0.0216 0.5528 0.4140 0.019 Uiso 1 1 calc R U . . .
H18B H 0.0108 0.6981 0.4857 0.019 Uiso 1 1 calc R U . . .
C19 C 0.1791(3) 0.6528(3) 0.46802(18) 0.0180(6) Uani 1 1 d . . . . .
H19A H 0.1929 0.6283 0.5227 0.022 Uiso 1 1 calc R U . . .
H19B H 0.2361 0.7456 0.4844 0.022 Uiso 1 1 calc R U . . .
C20 C 0.2208(3) 0.5606(3) 0.3980(2) 0.0231(6) Uani 1 1 d . . . . .
H20A H 0.1705 0.4670 0.3866 0.028 Uiso 1 1 calc R U . . .
H20B H 0.1976 0.5784 0.3411 0.028 Uiso 1 1 calc R U . . .
C21 C 0.3678(3) 0.5774(3) 0.4263(2) 0.0269(7) Uani 1 1 d . . . . .
H21A H 0.3885 0.5172 0.3783 0.040 Uiso 1 1 calc R U . . .
H21B H 0.3909 0.5560 0.4811 0.040 Uiso 1 1 calc R U . . .
H21C H 0.4184 0.6697 0.4375 0.040 Uiso 1 1 calc R U . . .
C22 C -0.1702(3) 0.4677(3) -0.01177(19) 0.0223(6) Uani 1 1 d . . . . .
C23 C -0.2143(4) 0.5090(3) -0.1479(2) 0.0315(7) Uani 1 1 d . . . . .
H23A H -0.2202 0.5822 -0.1704 0.047 Uiso 1 1 calc R U . . .
H23B H -0.3015 0.4423 -0.1682 0.047 Uiso 1 1 calc R U . . .
H23C H -0.1527 0.4679 -0.1709 0.047 Uiso 1 1 calc R U . . .
C24 C 0.1247(3) 0.9546(3) 0.44114(17) 0.0143(5) Uani 1 1 d . . . . .
C25 C 0.1456(3) 0.9722(3) 0.53240(18) 0.0164(5) Uani 1 1 d . . . . .
H25 H 0.1193 0.8976 0.5505 0.020 Uiso 1 1 calc R U . . .
C26 C 0.2047(3) 1.0984(3) 0.59592(18) 0.0164(5) Uani 1 1 d . . . . .
H26 H 0.2185 1.1099 0.6577 0.020 Uiso 1 1 calc R U . . .
C27 C 0.2444(3) 1.2095(3) 0.57046(18) 0.0154(5) Uani 1 1 d . . . . .
C28 C 0.2196(3) 1.1900(3) 0.47879(18) 0.0162(5) Uani 1 1 d . . . . .
H28 H 0.2445 1.2655 0.4612 0.019 Uiso 1 1 calc R U . . .
C29 C 0.1597(3) 1.0641(3) 0.41180(17) 0.0146(5) Uani 1 1 d . . . . .
C30 C 0.3103(3) 1.3454(3) 0.63913(18) 0.0176(6) Uani 1 1 d . . . . .
C31 C 0.3768(3) 1.3634(3) 0.7275(2) 0.0254(7) Uani 1 1 d . . . . .
H31 H 0.3791 1.2878 0.7445 0.030 Uiso 1 1 calc R U . . .
C32 C 0.4395(3) 1.4904(3) 0.7908(2) 0.0322(8) Uani 1 1 d . . . . .
H32 H 0.4830 1.5005 0.8507 0.039 Uiso 1 1 calc R U . . .
C33 C 0.4392(3) 1.6017(3) 0.7675(2) 0.0312(7) Uani 1 1 d . . . . .
H33 H 0.4834 1.6883 0.8107 0.037 Uiso 1 1 calc R U . . .
C34 C 0.3741(3) 1.5860(3) 0.6806(2) 0.0272(7) Uani 1 1 d . . . . .
H34 H 0.3736 1.6623 0.6640 0.033 Uiso 1 1 calc R U . . .
C35 C 0.3091(3) 1.4590(3) 0.6172(2) 0.0210(6) Uani 1 1 d . . . . .
H35 H 0.2631 1.4498 0.5580 0.025 Uiso 1 1 calc R U . . .
C36 C -0.1030(3) 1.1391(3) 0.29428(19) 0.0213(6) Uani 1 1 d . . . . .
C37 C -0.2496(3) 1.1150(3) 0.2634(2) 0.0319(7) Uani 1 1 d . . . . .
H37A H -0.2686 1.1679 0.2255 0.048 Uiso 1 1 calc R U . . .
H37B H -0.2808 1.1411 0.3157 0.048 Uiso 1 1 calc R U . . .
H37C H -0.2946 1.0202 0.2290 0.048 Uiso 1 1 calc R U . . .
C38 C 0.6844(9) 0.7638(12) 0.0832(7) 0.059(3) Uani 0.5 1 d . . P A 1
H38A H 0.7396 0.8332 0.1414 0.071 Uiso 0.5 1 calc R U P A 1
H38B H 0.7064 0.6808 0.0808 0.071 Uiso 0.5 1 calc R U P A 1
Cl1 Cl 0.7220(2) 0.8141(3) -0.00369(16) 0.0606(6) Uani 0.5 1 d . . P A 1
Cl2 Cl 0.5168(2) 0.7357(3) 0.0777(2) 0.0705(7) Uani 0.5 1 d . . P A 1
C39 C 0.4188(9) 0.1846(8) -0.0298(6) 0.112(6) Uani 0.5 1 d G . P B -2
C40 C 0.5215(9) 0.1488(9) -0.0564(6) 0.085(4) Uani 0.5 1 d G . P B -2
H40 H 0.5767 0.2049 -0.0779 0.102 Uiso 0.5 1 calc R U P B -2
C41 C 0.5434(9) 0.0311(11) -0.0516(8) 0.183(12) Uani 0.5 1 d G . P B -2
H41 H 0.6136 0.0067 -0.0697 0.219 Uiso 0.5 1 calc R U P B -2
C42 C 0.4625(10) -0.0509(10) -0.0202(8) 0.150(9) Uani 0.5 1 d G . P B -2
H42 H 0.4775 -0.1314 -0.0169 0.180 Uiso 0.5 1 calc R U P B -2
C43 C 0.3598(8) -0.0152(9) 0.0064(7) 0.115(6) Uani 0.5 1 d G . P B -2
H43 H 0.3046 -0.0712 0.0278 0.138 Uiso 0.5 1 calc R U P B -2
C44 C 0.3379(7) 0.1026(9) 0.0015(5) 0.078(3) Uani 0.5 1 d G . P B -2
H44 H 0.2677 0.1270 0.0197 0.093 Uiso 0.5 1 calc R U P B -2
C45 C 0.408(2) 0.3195(19) -0.0445(9) 0.145(9) Uani 0.5 1 d . . P B -2
H45A H 0.3611 0.3005 -0.1074 0.217 Uiso 0.5 1 calc R U P B -2
H45B H 0.4969 0.3816 -0.0290 0.217 Uiso 0.5 1 calc R U P B -2
H45C H 0.3603 0.3594 -0.0060 0.217 Uiso 0.5 1 calc R U P B -2
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
Os 0.02128(6) 0.01133(5) 0.01065(5) 0.00199(4) 0.00599(4) 0.00375(4)
O1 0.0448(15) 0.0217(11) 0.0194(11) -0.0027(9) 0.0060(10) 0.0018(11)
O2 0.0414(14) 0.0234(11) 0.0124(10) 0.0011(9) 0.0035(9) 0.0000(10)
O3 0.0237(11) 0.0194(10) 0.0206(10) 0.0092(8) 0.0075(9) 0.0068(9)
O4 0.0339(13) 0.0205(11) 0.0274(11) 0.0053(9) 0.0112(10) 0.0091(10)
N5 0.0167(12) 0.0127(11) 0.0114(10) 0.0019(9) 0.0033(9) 0.0041(9)
N8 0.0153(11) 0.0123(10) 0.0140(11) 0.0039(9) 0.0044(9) 0.0044(9)
C1 0.0344(17) 0.0196(14) 0.0156(14) 0.0074(11) 0.0119(13) 0.0048(13)
C2 0.0328(17) 0.0139(13) 0.0167(13) 0.0044(11) 0.0122(13) 0.0044(12)
C3 0.0243(15) 0.0165(13) 0.0143(13) 0.0022(11) 0.0078(12) -0.0022(12)
C4 0.0241(15) 0.0175(14) 0.0210(14) 0.0050(11) 0.0130(12) 0.0041(12)
C5 0.0269(16) 0.0160(13) 0.0182(14) 0.0024(11) 0.0132(12) 0.0045(12)
C6 0.0361(18) 0.0201(14) 0.0104(13) 0.0031(11) 0.0097(12) 0.0050(13)
C7 0.041(2) 0.0287(17) 0.0181(14) 0.0107(13) 0.0096(14) 0.0123(15)
C8 0.0212(16) 0.0275(16) 0.0287(16) 0.0070(13) 0.0123(13) 0.0068(13)
C9 0.033(2) 0.0244(17) 0.056(2) 0.0118(17) 0.0041(18) 0.0112(15)
C10 0.0298(18) 0.0279(17) 0.0318(18) 0.0060(14) 0.0031(15) 0.0037(14)
C11 0.0116(13) 0.0140(12) 0.0156(12) 0.0045(10) 0.0057(10) 0.0046(10)
C12 0.0148(13) 0.0159(13) 0.0124(12) 0.0025(10) 0.0043(10) 0.0042(11)
C13 0.0198(15) 0.0146(13) 0.0188(13) 0.0039(11) 0.0071(12) 0.0022(12)
C14 0.0183(14) 0.0150(13) 0.0207(14) -0.0004(11) 0.0060(12) 0.0002(11)
C15 0.0183(14) 0.0192(14) 0.0157(13) 0.0001(11) 0.0041(11) 0.0006(12)
C16 0.0201(14) 0.0177(13) 0.0135(13) 0.0032(11) 0.0050(11) 0.0023(11)
C17 0.0146(13) 0.0141(12) 0.0134(12) 0.0013(10) 0.0053(10) 0.0020(10)
C18 0.0195(14) 0.0142(13) 0.0164(13) 0.0061(11) 0.0070(11) 0.0056(11)
C19 0.0206(15) 0.0164(13) 0.0165(13) 0.0057(11) 0.0037(11) 0.0067(11)
C20 0.0222(15) 0.0208(15) 0.0239(15) 0.0026(12) 0.0064(12) 0.0088(12)
C21 0.0248(16) 0.0261(16) 0.0313(17) 0.0082(14) 0.0092(14) 0.0117(13)
C22 0.0207(15) 0.0222(15) 0.0168(14) 0.0006(12) 0.0060(12) 0.0008(12)
C23 0.0375(19) 0.0319(18) 0.0126(14) 0.0012(13) 0.0014(13) 0.0016(15)
C24 0.0148(13) 0.0134(12) 0.0144(12) 0.0029(10) 0.0051(10) 0.0053(10)
C25 0.0198(14) 0.0167(13) 0.0148(13) 0.0069(11) 0.0052(11) 0.0081(11)
C26 0.0164(14) 0.0210(14) 0.0110(12) 0.0036(11) 0.0033(10) 0.0076(11)
C27 0.0146(13) 0.0164(13) 0.0135(12) 0.0013(10) 0.0046(10) 0.0059(11)
C28 0.0194(14) 0.0135(13) 0.0158(13) 0.0039(10) 0.0073(11) 0.0050(11)
C29 0.0146(13) 0.0160(13) 0.0128(12) 0.0042(10) 0.0051(10) 0.0042(11)
C30 0.0145(13) 0.0185(14) 0.0160(13) -0.0011(11) 0.0057(11) 0.0059(11)
C31 0.0257(16) 0.0267(16) 0.0185(14) 0.0015(12) 0.0021(12) 0.0104(13)
C32 0.0275(18) 0.0362(19) 0.0189(15) -0.0056(14) -0.0013(13) 0.0103(15)
C33 0.0244(17) 0.0237(16) 0.0304(17) -0.0078(13) 0.0057(14) 0.0033(13)
C34 0.0263(17) 0.0170(14) 0.0316(17) -0.0002(13) 0.0111(14) 0.0028(13)
C35 0.0196(15) 0.0207(14) 0.0196(14) 0.0023(12) 0.0076(12) 0.0044(12)
C36 0.0281(16) 0.0248(15) 0.0169(14) 0.0108(12) 0.0109(12) 0.0110(13)
C37 0.0326(19) 0.0307(18) 0.041(2) 0.0158(15) 0.0159(16) 0.0162(15)
C38 0.041(5) 0.075(7) 0.056(6) 0.013(5) 0.011(5) 0.018(5)
Cl1 0.0523(13) 0.0678(15) 0.0529(13) 0.0094(11) 0.0080(11) 0.0239(12)
Cl2 0.0404(12) 0.0892(19) 0.0911(19) 0.0403(16) 0.0189(13) 0.0268(13)
C39 0.112(12) 0.147(14) 0.034(6) 0.003(7) 0.014(7) 0.004(11)
C40 0.048(6) 0.095(9) 0.118(11) 0.044(8) 0.037(7) 0.013(6)
C41 0.113(15) 0.37(4) 0.154(18) 0.15(2) 0.091(14) 0.11(2)
C42 0.18(2) 0.15(2) 0.154(19) 0.070(17) 0.137(18) 0.023(15)
C43 0.119(12) 0.205(18) 0.110(11) 0.106(13) 0.086(10) 0.101(13)
C44 0.054(7) 0.083(8) 0.069(7) 0.009(6) 0.003(6) 0.007(6)
C45 0.20(2) 0.159(17) 0.062(9) -0.010(10) -0.004(11) 0.138(17)
_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
Os C29 2.077(3) . ?
Os N5 2.086(2) . ?
Os O3 2.099(2) . ?
Os C3 2.148(3) . ?
Os C5 2.167(3) . ?
Os C2 2.188(3) . ?
Os C4 2.198(3) . ?
Os C1 2.243(3) . ?
Os C6 2.265(3) . ?
O1 C22 1.206(4) . ?
O2 C22 1.340(4) . ?
O2 C23 1.446(3) . ?
O3 C36 1.292(3) . ?
O4 C36 1.231(4) . ?
N5 C11 1.338(3) . ?
N5 C17 1.385(3) . ?
N8 C11 1.371(3) . ?
N8 C12 1.379(3) . ?
N8 C18 1.473(3) . ?
C1 C6 1.418(4) . ?
C1 C2 1.432(4) . ?
C1 C7 1.494(4) . ?
C2 C3 1.414(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.430(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.421(4) . ?
C4 C8 1.518(4) . ?
C5 C6 1.426(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C10 1.517(4) . ?
C8 C9 1.533(5) . ?
C8 H8 1.0000 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C24 1.447(4) . ?
C12 C13 1.398(4) . ?
C12 C17 1.403(4) . ?
C13 C14 1.383(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.408(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.391(4) . ?
C15 C22 1.484(4) . ?
C16 C17 1.389(4) . ?
C16 H16 0.9500 . ?
C18 C19 1.526(4) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.530(4) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.527(4) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.402(4) . ?
C24 C29 1.415(4) . ?
C25 C26 1.382(4) . ?
C25 H25 0.9500 . ?
C26 C27 1.400(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.401(4) . ?
C27 C30 1.492(4) . ?
C28 C29 1.402(4) . ?
C28 H28 0.9500 . ?
C30 C35 1.393(4) . ?
C30 C31 1.398(4) . ?
C31 C32 1.390(4) . ?
C31 H31 0.9500 . ?
C32 C33 1.377(5) . ?
C32 H32 0.9500 . ?
C33 C34 1.380(5) . ?
C33 H33 0.9500 . ?
C34 C35 1.394(4) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 C37 1.509(5) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 Cl1 1.746(11) . ?
C38 Cl2 1.767(10) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.3900 . ?
C39 C44 1.3900 . ?
C39 C45 1.591(18) . ?
C40 C41 1.3900 . ?
C40 H40 0.9500 . ?
C41 C42 1.3900 . ?
C41 H41 0.9500 . ?
C42 C43 1.3900 . ?
C42 H42 0.9500 . ?
C43 C44 1.3900 . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 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
C29 Os N5 76.20(9) . . ?
C29 Os O3 88.85(9) . . ?
N5 Os O3 81.81(8) . . ?
C29 Os C3 90.67(10) . . ?
N5 Os C3 138.80(10) . . ?
O3 Os C3 137.63(10) . . ?
C29 Os C5 133.36(11) . . ?
N5 Os C5 92.87(10) . . ?
O3 Os C5 135.02(10) . . ?
C3 Os C5 68.05(11) . . ?
C29 Os C2 108.36(11) . . ?
N5 Os C2 173.27(10) . . ?
O3 Os C2 102.98(10) . . ?
C3 Os C2 38.06(11) . . ?
C5 Os C2 80.40(11) . . ?
C29 Os C4 100.78(11) . . ?
N5 Os C4 105.25(10) . . ?
O3 Os C4 169.13(9) . . ?
C3 Os C4 38.40(11) . . ?
C5 Os C4 37.98(11) . . ?
C2 Os C4 69.33(11) . . ?
C29 Os C1 143.11(11) . . ?
N5 Os C1 139.23(10) . . ?
O3 Os C1 87.66(10) . . ?
C3 Os C1 68.28(11) . . ?
C5 Os C1 67.69(11) . . ?
C2 Os C1 37.68(11) . . ?
C4 Os C1 81.61(11) . . ?
C29 Os C6 168.82(11) . . ?
N5 Os C6 107.79(10) . . ?
O3 Os C6 101.99(10) . . ?
C3 Os C6 79.49(11) . . ?
C5 Os C6 37.47(11) . . ?
C2 Os C6 66.80(10) . . ?
C4 Os C6 68.18(11) . . ?
C1 Os C6 36.65(10) . . ?
C22 O2 C23 115.2(2) . . ?
C36 O3 Os 125.70(19) . . ?
C11 N5 C17 107.0(2) . . ?
C11 N5 Os 117.90(17) . . ?
C17 N5 Os 134.88(18) . . ?
C11 N8 C12 107.2(2) . . ?
C11 N8 C18 127.7(2) . . ?
C12 N8 C18 124.2(2) . . ?
C6 C1 C2 118.8(3) . . ?
C6 C1 C7 120.7(3) . . ?
C2 C1 C7 120.5(3) . . ?
C6 C1 Os 72.50(16) . . ?
C2 C1 Os 69.07(16) . . ?
C7 C1 Os 127.5(2) . . ?
C3 C2 C1 120.1(3) . . ?
C3 C2 Os 69.42(16) . . ?
C1 C2 Os 73.26(16) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
Os C2 H2 129.8 . . ?
C2 C3 C4 122.6(3) . . ?
C2 C3 Os 72.52(17) . . ?
C4 C3 Os 72.71(17) . . ?
C2 C3 H3 118.7 . . ?
C4 C3 H3 118.7 . . ?
Os C3 H3 128.5 . . ?
C5 C4 C3 115.7(3) . . ?
C5 C4 C8 121.2(3) . . ?
C3 C4 C8 123.0(3) . . ?
C5 C4 Os 69.80(16) . . ?
C3 C4 Os 68.89(16) . . ?
C8 C4 Os 131.3(2) . . ?
C4 C5 C6 123.0(3) . . ?
C4 C5 Os 72.22(16) . . ?
C6 C5 Os 75.02(16) . . ?
C4 C5 H5 118.5 . . ?
C6 C5 H5 118.5 . . ?
Os C5 H5 126.2 . . ?
C1 C6 C5 119.5(3) . . ?
C1 C6 Os 70.85(16) . . ?
C5 C6 Os 67.52(15) . . ?
C1 C6 H6 120.2 . . ?
C5 C6 H6 120.2 . . ?
Os C6 H6 134.9 . . ?
C1 C7 H7A 109.5 . . ?
C1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C10 C8 C4 113.6(3) . . ?
C10 C8 C9 108.7(3) . . ?
C4 C8 C9 112.8(3) . . ?
C10 C8 H8 107.1 . . ?
C4 C8 H8 107.1 . . ?
C9 C8 H8 107.1 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N5 C11 N8 110.9(2) . . ?
N5 C11 C24 116.2(2) . . ?
N8 C11 C24 132.9(2) . . ?
N8 C12 C13 131.6(2) . . ?
N8 C12 C17 106.7(2) . . ?
C13 C12 C17 121.7(2) . . ?
C14 C13 C12 117.0(3) . . ?
C14 C13 H13 121.5 . . ?
C12 C13 H13 121.5 . . ?
C13 C14 C15 121.4(3) . . ?
C13 C14 H14 119.3 . . ?
C15 C14 H14 119.3 . . ?
C16 C15 C14 121.4(3) . . ?
C16 C15 C22 121.1(3) . . ?
C14 C15 C22 117.5(3) . . ?
C17 C16 C15 117.4(3) . . ?
C17 C16 H16 121.3 . . ?
C15 C16 H16 121.3 . . ?
N5 C17 C16 130.8(3) . . ?
N5 C17 C12 108.1(2) . . ?
C16 C17 C12 121.1(2) . . ?
N8 C18 C19 111.1(2) . . ?
N8 C18 H18A 109.4 . . ?
C19 C18 H18A 109.4 . . ?
N8 C18 H18B 109.4 . . ?
C19 C18 H18B 109.4 . . ?
H18A C18 H18B 108.0 . . ?
C18 C19 C20 113.1(2) . . ?
C18 C19 H19A 109.0 . . ?
C20 C19 H19A 109.0 . . ?
C18 C19 H19B 109.0 . . ?
C20 C19 H19B 109.0 . . ?
H19A C19 H19B 107.8 . . ?
C21 C20 C19 113.4(3) . . ?
C21 C20 H20A 108.9 . . ?
C19 C20 H20A 108.9 . . ?
C21 C20 H20B 108.9 . . ?
C19 C20 H20B 108.9 . . ?
H20A C20 H20B 107.7 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O1 C22 O2 123.0(3) . . ?
O1 C22 C15 124.7(3) . . ?
O2 C22 C15 112.3(2) . . ?
O2 C23 H23A 109.5 . . ?
O2 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
O2 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 C29 121.4(2) . . ?
C25 C24 C11 126.6(2) . . ?
C29 C24 C11 111.9(2) . . ?
C26 C25 C24 119.9(3) . . ?
C26 C25 H25 120.1 . . ?
C24 C25 H25 120.1 . . ?
C25 C26 C27 120.9(2) . . ?
C25 C26 H26 119.6 . . ?
C27 C26 H26 119.6 . . ?
C26 C27 C28 118.3(2) . . ?
C26 C27 C30 120.9(2) . . ?
C28 C27 C30 120.8(2) . . ?
C27 C28 C29 122.9(2) . . ?
C27 C28 H28 118.5 . . ?
C29 C28 H28 118.5 . . ?
C28 C29 C24 116.5(2) . . ?
C28 C29 Os 125.9(2) . . ?
C24 C29 Os 117.53(19) . . ?
C35 C30 C31 117.6(3) . . ?
C35 C30 C27 121.1(3) . . ?
C31 C30 C27 121.3(3) . . ?
C32 C31 C30 121.0(3) . . ?
C32 C31 H31 119.5 . . ?
C30 C31 H31 119.5 . . ?
C33 C32 C31 120.6(3) . . ?
C33 C32 H32 119.7 . . ?
C31 C32 H32 119.7 . . ?
C32 C33 C34 119.3(3) . . ?
C32 C33 H33 120.4 . . ?
C34 C33 H33 120.4 . . ?
C33 C34 C35 120.4(3) . . ?
C33 C34 H34 119.8 . . ?
C35 C34 H34 119.8 . . ?
C30 C35 C34 121.1(3) . . ?
C30 C35 H35 119.5 . . ?
C34 C35 H35 119.5 . . ?
O4 C36 O3 126.7(3) . . ?
O4 C36 C37 120.3(3) . . ?
O3 C36 C37 112.9(3) . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
Cl1 C38 Cl2 112.7(6) . . ?
Cl1 C38 H38A 109.0 . . ?
Cl2 C38 H38A 109.0 . . ?
Cl1 C38 H38B 109.0 . . ?
Cl2 C38 H38B 109.0 . . ?
H38A C38 H38B 107.8 . . ?
C40 C39 C44 120.0 . . ?
C40 C39 C45 111.6(10) . . ?
C44 C39 C45 128.4(10) . . ?
C39 C40 C41 120.0 . . ?
C39 C40 H40 120.0 . . ?
C41 C40 H40 120.0 . . ?
C42 C41 C40 120.0 . . ?
C42 C41 H41 120.0 . . ?
C40 C41 H41 120.0 . . ?
C41 C42 C43 120.0 . . ?
C41 C42 H42 120.0 . . ?
C43 C42 H42 120.0 . . ?
C42 C43 C44 120.0 . . ?
C42 C43 H43 120.0 . . ?
C44 C43 H43 120.0 . . ?
C43 C44 C39 120.0 . . ?
C43 C44 H44 120.0 . . ?
C39 C44 H44 120.0 . . ?
C39 C45 H45A 109.5 . . ?
C39 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C39 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -1.5(4) . . . . ?
C7 C1 C2 C3 175.3(3) . . . . ?
Os C1 C2 C3 53.2(2) . . . . ?
C6 C1 C2 Os -54.8(2) . . . . ?
C7 C1 C2 Os 122.0(3) . . . . ?
C1 C2 C3 C4 0.1(4) . . . . ?
Os C2 C3 C4 55.2(2) . . . . ?
C1 C2 C3 Os -55.0(2) . . . . ?
C2 C3 C4 C5 -1.7(4) . . . . ?
Os C3 C4 C5 53.3(2) . . . . ?
C2 C3 C4 C8 178.6(3) . . . . ?
Os C3 C4 C8 -126.3(3) . . . . ?
C2 C3 C4 Os -55.1(2) . . . . ?
C3 C4 C5 C6 5.0(4) . . . . ?
C8 C4 C5 C6 -175.4(3) . . . . ?
Os C4 C5 C6 57.8(3) . . . . ?
C3 C4 C5 Os -52.9(2) . . . . ?
C8 C4 C5 Os 126.8(3) . . . . ?
C2 C1 C6 C5 4.5(4) . . . . ?
C7 C1 C6 C5 -172.2(3) . . . . ?
Os C1 C6 C5 -48.6(2) . . . . ?
C2 C1 C6 Os 53.1(2) . . . . ?
C7 C1 C6 Os -123.7(3) . . . . ?
C4 C5 C6 C1 -6.5(4) . . . . ?
Os C5 C6 C1 50.0(2) . . . . ?
C4 C5 C6 Os -56.6(2) . . . . ?
C5 C4 C8 C10 -168.0(3) . . . . ?
C3 C4 C8 C10 11.7(4) . . . . ?
Os C4 C8 C10 -78.3(3) . . . . ?
C5 C4 C8 C9 -43.7(4) . . . . ?
C3 C4 C8 C9 135.9(3) . . . . ?
Os C4 C8 C9 46.0(4) . . . . ?
C17 N5 C11 N8 0.9(3) . . . . ?
Os N5 C11 N8 -174.32(16) . . . . ?
C17 N5 C11 C24 -179.5(2) . . . . ?
Os N5 C11 C24 5.3(3) . . . . ?
C12 N8 C11 N5 -0.6(3) . . . . ?
C18 N8 C11 N5 168.9(2) . . . . ?
C12 N8 C11 C24 179.9(3) . . . . ?
C18 N8 C11 C24 -10.6(5) . . . . ?
C11 N8 C12 C13 179.0(3) . . . . ?
C18 N8 C12 C13 8.9(5) . . . . ?
C11 N8 C12 C17 0.1(3) . . . . ?
C18 N8 C12 C17 -170.0(2) . . . . ?
N8 C12 C13 C14 -179.6(3) . . . . ?
C17 C12 C13 C14 -0.9(4) . . . . ?
C12 C13 C14 C15 0.5(4) . . . . ?
C13 C14 C15 C16 0.1(4) . . . . ?
C13 C14 C15 C22 179.4(3) . . . . ?
C14 C15 C16 C17 -0.4(4) . . . . ?
C22 C15 C16 C17 -179.7(3) . . . . ?
C11 N5 C17 C16 -179.9(3) . . . . ?
Os N5 C17 C16 -5.9(5) . . . . ?
C11 N5 C17 C12 -0.9(3) . . . . ?
Os N5 C17 C12 173.19(19) . . . . ?
C15 C16 C17 N5 179.0(3) . . . . ?
C15 C16 C17 C12 0.0(4) . . . . ?
N8 C12 C17 N5 0.5(3) . . . . ?
C13 C12 C17 N5 -178.6(2) . . . . ?
N8 C12 C17 C16 179.7(2) . . . . ?
C13 C12 C17 C16 0.6(4) . . . . ?
C11 N8 C18 C19 -68.3(3) . . . . ?
C12 N8 C18 C19 99.7(3) . . . . ?
N8 C18 C19 C20 -66.9(3) . . . . ?
C18 C19 C20 C21 173.7(2) . . . . ?
C23 O2 C22 O1 -0.3(4) . . . . ?
C23 O2 C22 C15 -179.4(3) . . . . ?
C16 C15 C22 O1 171.2(3) . . . . ?
C14 C15 C22 O1 -8.2(5) . . . . ?
C16 C15 C22 O2 -9.8(4) . . . . ?
C14 C15 C22 O2 170.8(3) . . . . ?
N5 C11 C24 C25 174.5(3) . . . . ?
N8 C11 C24 C25 -6.0(5) . . . . ?
N5 C11 C24 C29 -1.9(3) . . . . ?
N8 C11 C24 C29 177.6(3) . . . . ?
C29 C24 C25 C26 -1.7(4) . . . . ?
C11 C24 C25 C26 -177.8(3) . . . . ?
C24 C25 C26 C27 -0.1(4) . . . . ?
C25 C26 C27 C28 1.7(4) . . . . ?
C25 C26 C27 C30 -178.9(2) . . . . ?
C26 C27 C28 C29 -1.5(4) . . . . ?
C30 C27 C28 C29 179.1(2) . . . . ?
C27 C28 C29 C24 -0.2(4) . . . . ?
C27 C28 C29 Os -179.4(2) . . . . ?
C25 C24 C29 C28 1.8(4) . . . . ?
C11 C24 C29 C28 178.5(2) . . . . ?
C25 C24 C29 Os -178.9(2) . . . . ?
C11 C24 C29 Os -2.2(3) . . . . ?
C26 C27 C30 C35 -157.3(3) . . . . ?
C28 C27 C30 C35 22.1(4) . . . . ?
C26 C27 C30 C31 23.4(4) . . . . ?
C28 C27 C30 C31 -157.2(3) . . . . ?
C35 C30 C31 C32 -0.2(4) . . . . ?
C27 C30 C31 C32 179.1(3) . . . . ?
C30 C31 C32 C33 -1.0(5) . . . . ?
C31 C32 C33 C34 1.0(5) . . . . ?
C32 C33 C34 C35 0.1(5) . . . . ?
C31 C30 C35 C34 1.3(4) . . . . ?
C27 C30 C35 C34 -178.0(3) . . . . ?
C33 C34 C35 C30 -1.3(5) . . . . ?
Os O3 C36 O4 -11.7(4) . . . . ?
Os O3 C36 C37 167.88(19) . . . . ?
C44 C39 C40 C41 0.0 . . . . ?
C45 C39 C40 C41 -177.8(9) . . . . ?
C39 C40 C41 C42 0.0 . . . . ?
C40 C41 C42 C43 0.0 . . . . ?
C41 C42 C43 C44 0.0 . . . . ?
C42 C43 C44 C39 0.0 . . . . ?
C40 C39 C44 C43 0.0 . . . . ?
C45 C39 C44 C43 177.4(11) . . . . ?
_refine_diff_density_max 2.004
_refine_diff_density_min -0.989
_refine_diff_density_rms 0.121
_shelx_res_file
;
jY85.res created by SHELXL-2014/7
TITL jY85 in P1 New: P-1
CELL 0.71073 10.9559 10.9932 16.2594 105.966 102.536 103.578
ZERR 2 0.0006 0.0006 0.0009 0.002 0.002 0.002
LATT 1
SFAC C H N O Os Cl
UNIT 82 90 4 8 2 2
LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!!
LIST 4
TEMP -173.150
SIZE 0.126 0.131 0.213
L.S. 6
FMAP 2
PLAN 20
ACTA
BOND $H
CONF
WGHT 0.011200 3.932300
FVAR 0.08952
OS 5 0.120211 1.024504 0.274580 11.00000 0.02128 0.01133 =
0.01065 0.00199 0.00599 0.00375
O1 4 -0.208588 0.349754 -0.053657 11.00000 0.04481 0.02170 =
0.01938 -0.00272 0.00599 0.00184
O2 4 -0.167909 0.560304 -0.050949 11.00000 0.04136 0.02339 =
0.01236 0.00112 0.00349 -0.00005
O3 4 -0.071136 1.032142 0.268134 11.00000 0.02375 0.01937 =
0.02063 0.00917 0.00748 0.00680
O4 4 -0.027417 1.252029 0.339103 11.00000 0.03395 0.02047 =
0.02741 0.00528 0.01124 0.00913
N5 3 0.041518 0.838921 0.284610 11.00000 0.01670 0.01267 =
0.01140 0.00190 0.00327 0.00411
N8 3 0.014160 0.700682 0.361876 11.00000 0.01525 0.01227 =
0.01400 0.00387 0.00443 0.00441
C1 1 0.115744 1.121754 0.169876 11.00000 0.03438 0.01965 =
0.01560 0.00735 0.01185 0.00485
C2 1 0.213175 1.207368 0.252871 11.00000 0.03280 0.01388 =
0.01672 0.00438 0.01222 0.00438
AFIX 43
H2 2 0.213005 1.295859 0.279351 11.00000 -1.20000
AFIX 0
C3 1 0.309648 1.160333 0.295460 11.00000 0.02429 0.01646 =
0.01433 0.00222 0.00778 -0.00222
AFIX 43
H3 2 0.373265 1.218735 0.350533 11.00000 -1.20000
AFIX 0
C4 1 0.315257 1.028361 0.258929 11.00000 0.02409 0.01752 =
0.02104 0.00500 0.01301 0.00412
C5 1 0.214999 0.945156 0.177827 11.00000 0.02691 0.01596 =
0.01817 0.00238 0.01321 0.00447
AFIX 43
H5 2 0.210847 0.854614 0.153804 11.00000 -1.20000
AFIX 0
C6 1 0.120277 0.991267 0.130792 11.00000 0.03614 0.02013 =
0.01041 0.00309 0.00967 0.00497
AFIX 43
H6 2 0.060664 0.934948 0.073693 11.00000 -1.20000
AFIX 0
C7 1 0.007322 1.166780 0.127925 11.00000 0.04108 0.02868 =
0.01806 0.01072 0.00959 0.01226
AFIX 137
H7A 2 0.031736 1.203635 0.083192 11.00000 -1.50000
H7B 2 -0.007296 1.235433 0.174326 11.00000 -1.50000
H7C 2 -0.073604 1.090813 0.098736 11.00000 -1.50000
AFIX 0
C8 1 0.420250 0.977892 0.303040 11.00000 0.02125 0.02750 =
0.02866 0.00696 0.01233 0.00675
AFIX 13
H8 2 0.482358 0.973158 0.266239 11.00000 -1.20000
AFIX 0
C9 1 0.364012 0.837291 0.304544 11.00000 0.03259 0.02444 =
0.05604 0.01177 0.00406 0.01116
AFIX 137
H9A 2 0.436430 0.805444 0.327002 11.00000 -1.50000
H9B 2 0.311889 0.777161 0.243660 11.00000 -1.50000
H9C 2 0.307759 0.839375 0.343933 11.00000 -1.50000
AFIX 0
C10 1 0.500897 1.069296 0.397724 11.00000 0.02976 0.02786 =
0.03184 0.00603 0.00306 0.00369
AFIX 137
H10A 2 0.566653 1.031270 0.422184 11.00000 -1.50000
H10B 2 0.442646 1.078629 0.435461 11.00000 -1.50000
H10C 2 0.545483 1.157026 0.396683 11.00000 -1.50000
AFIX 0
C11 1 0.060604 0.830367 0.366658 11.00000 0.01164 0.01404 =
0.01561 0.00449 0.00569 0.00459
C12 1 -0.038090 0.623581 0.272212 11.00000 0.01477 0.01588 =
0.01238 0.00251 0.00430 0.00419
C13 1 -0.096414 0.486027 0.229109 11.00000 0.01981 0.01460 =
0.01883 0.00390 0.00712 0.00215
AFIX 43
H13 2 -0.106509 0.427082 0.262071 11.00000 -1.20000
AFIX 0
C14 1 -0.138745 0.439637 0.136335 11.00000 0.01826 0.01498 =
0.02074 -0.00036 0.00597 0.00023
AFIX 43
H14 2 -0.179506 0.346800 0.104830 11.00000 -1.20000
AFIX 0
C15 1 -0.122747 0.526992 0.087567 11.00000 0.01825 0.01921 =
0.01570 0.00014 0.00414 0.00058
C16 1 -0.063536 0.663644 0.130614 11.00000 0.02011 0.01768 =
0.01345 0.00317 0.00496 0.00233
AFIX 43
H16 2 -0.052362 0.722397 0.097597 11.00000 -1.20000
AFIX 0
C17 1 -0.021394 0.710796 0.223783 11.00000 0.01460 0.01415 =
0.01339 0.00125 0.00526 0.00199
C18 1 0.035542 0.646475 0.435262 11.00000 0.01955 0.01423 =
0.01638 0.00612 0.00699 0.00557
AFIX 23
H18A 2 -0.021589 0.552754 0.413984 11.00000 -1.20000
H18B 2 0.010830 0.698066 0.485699 11.00000 -1.20000
AFIX 0
C19 1 0.179146 0.652841 0.468015 11.00000 0.02056 0.01641 =
0.01651 0.00570 0.00369 0.00667
AFIX 23
H19A 2 0.192938 0.628279 0.522729 11.00000 -1.20000
H19B 2 0.236134 0.745616 0.484442 11.00000 -1.20000
AFIX 0
C20 1 0.220794 0.560598 0.397998 11.00000 0.02224 0.02085 =
0.02385 0.00260 0.00639 0.00877
AFIX 23
H20A 2 0.170549 0.467044 0.386595 11.00000 -1.20000
H20B 2 0.197643 0.578378 0.341073 11.00000 -1.20000
AFIX 0
C21 1 0.367810 0.577372 0.426260 11.00000 0.02484 0.02609 =
0.03125 0.00817 0.00922 0.01172
AFIX 137
H21A 2 0.388542 0.517231 0.378308 11.00000 -1.50000
H21B 2 0.390863 0.555954 0.481116 11.00000 -1.50000
H21C 2 0.418370 0.669695 0.437494 11.00000 -1.50000
AFIX 0
C22 1 -0.170201 0.467686 -0.011768 11.00000 0.02070 0.02225 =
0.01678 0.00060 0.00597 0.00078
C23 1 -0.214331 0.509049 -0.147937 11.00000 0.03749 0.03189 =
0.01260 0.00116 0.00137 0.00156
AFIX 137
H23A 2 -0.220219 0.582246 -0.170375 11.00000 -1.50000
H23B 2 -0.301504 0.442305 -0.168211 11.00000 -1.50000
H23C 2 -0.152728 0.467863 -0.170948 11.00000 -1.50000
AFIX 0
C24 1 0.124698 0.954572 0.441143 11.00000 0.01478 0.01335 =
0.01439 0.00292 0.00507 0.00529
C25 1 0.145636 0.972230 0.532397 11.00000 0.01984 0.01673 =
0.01476 0.00685 0.00519 0.00808
AFIX 43
H25 2 0.119295 0.897596 0.550546 11.00000 -1.20000
AFIX 0
C26 1 0.204676 1.098422 0.595923 11.00000 0.01638 0.02105 =
0.01103 0.00357 0.00334 0.00765
AFIX 43
H26 2 0.218475 1.109916 0.657682 11.00000 -1.20000
AFIX 0
C27 1 0.244401 1.209502 0.570458 11.00000 0.01462 0.01642 =
0.01348 0.00126 0.00461 0.00586
C28 1 0.219616 1.190020 0.478786 11.00000 0.01945 0.01346 =
0.01582 0.00395 0.00727 0.00502
AFIX 43
H28 2 0.244512 1.265491 0.461207 11.00000 -1.20000
AFIX 0
C29 1 0.159698 1.064099 0.411805 11.00000 0.01463 0.01602 =
0.01282 0.00415 0.00512 0.00418
C30 1 0.310314 1.345358 0.639127 11.00000 0.01455 0.01851 =
0.01600 -0.00108 0.00574 0.00594
C31 1 0.376781 1.363404 0.727492 11.00000 0.02565 0.02667 =
0.01852 0.00146 0.00209 0.01042
AFIX 43
H31 2 0.379096 1.287753 0.744523 11.00000 -1.20000
AFIX 0
C32 1 0.439532 1.490403 0.790805 11.00000 0.02750 0.03619 =
0.01886 -0.00557 -0.00128 0.01034
AFIX 43
H32 2 0.483018 1.500520 0.850723 11.00000 -1.20000
AFIX 0
C33 1 0.439246 1.601658 0.767484 11.00000 0.02445 0.02374 =
0.03045 -0.00785 0.00572 0.00327
AFIX 43
H33 2 0.483418 1.688259 0.810716 11.00000 -1.20000
AFIX 0
C34 1 0.374103 1.585992 0.680635 11.00000 0.02633 0.01701 =
0.03162 -0.00021 0.01112 0.00279
AFIX 43
H34 2 0.373592 1.662251 0.663987 11.00000 -1.20000
AFIX 0
C35 1 0.309057 1.459015 0.617188 11.00000 0.01957 0.02071 =
0.01958 0.00232 0.00763 0.00441
AFIX 43
H35 2 0.263096 1.449831 0.557989 11.00000 -1.20000
AFIX 0
C36 1 -0.103032 1.139145 0.294285 11.00000 0.02809 0.02479 =
0.01694 0.01083 0.01088 0.01095
C37 1 -0.249597 1.114955 0.263412 11.00000 0.03265 0.03067 =
0.04072 0.01583 0.01590 0.01615
AFIX 137
H37A 2 -0.268591 1.167892 0.225503 11.00000 -1.50000
H37B 2 -0.280758 1.141088 0.315730 11.00000 -1.50000
H37C 2 -0.294622 1.020175 0.228954 11.00000 -1.50000
AFIX 0
PART 1
C38 1 0.684410 0.763789 0.083240 10.50000 0.04074 0.07458 =
0.05551 0.01304 0.01130 0.01842
AFIX 23
H38A 2 0.739616 0.833178 0.141396 10.50000 -1.20000
H38B 2 0.706427 0.680783 0.080817 10.50000 -1.20000
AFIX 0
CL1 6 0.722003 0.814104 -0.003691 10.50000 0.05232 0.06778 =
0.05294 0.00943 0.00800 0.02390
CL2 6 0.516762 0.735718 0.077691 10.50000 0.04043 0.08918 =
0.09111 0.04025 0.01894 0.02679
PART -2
AFIX 66 1.3900
C39 1 0.418777 0.184570 -0.029848 10.50000 0.11220 0.14711 =
0.03377 0.00257 0.01400 0.00403
C40 1 0.521484 0.148842 -0.056410 10.50000 0.04800 0.09528 =
0.11763 0.04444 0.03720 0.01292
AFIX 43
H40 2 0.576730 0.204889 -0.077866 10.50000 -1.20000
AFIX 65
C41 1 0.543355 0.031108 -0.051578 10.50000 0.11335 0.36682 =
0.15364 0.15340 0.09054 0.10776
AFIX 43
H41 2 0.613550 0.006690 -0.069732 10.50000 -1.20000
AFIX 65
C42 1 0.462521 -0.050899 -0.020184 10.50000 0.17969 0.15473 =
0.15428 0.07006 0.13708 0.02299
AFIX 43
H42 2 0.477470 -0.131364 -0.016882 10.50000 -1.20000
AFIX 65
C43 1 0.359814 -0.015172 0.006378 10.50000 0.11866 0.20464 =
0.10960 0.10584 0.08621 0.10092
AFIX 43
H43 2 0.304568 -0.071220 0.027834 10.50000 -1.20000
AFIX 65
C44 1 0.337940 0.102561 0.001547 10.50000 0.05376 0.08302 =
0.06908 0.00901 0.00313 0.00690
AFIX 43
H44 2 0.267745 0.126979 0.019701 10.50000 -1.20000
AFIX 0
C45 1 0.408251 0.319462 -0.044488 10.50000 0.20374 0.15920 =
0.06153 -0.01035 -0.00402 0.13751
AFIX 137
H45A 2 0.361116 0.300498 -0.107439 10.50000 -1.50000
H45B 2 0.496872 0.381565 -0.029033 10.50000 -1.50000
H45C 2 0.360283 0.359406 -0.006009 10.50000 -1.50000
PART 0
AFIX 0
HKLF 4
REM jY85 in P1 New: P-1
REM R1 = 0.0267 for 7910 Fo > 4sig(Fo) and 0.0333 for all 8746 data
REM 482 parameters refined using 0 restraints
END
WGHT 0.0112 3.9324
REM Highest difference peak 2.004, deepest hole -0.989, 1-sigma level 0.121
Q1 1 -0.3647 0.9242 0.1741 11.00000 0.05 2.00
Q2 1 0.0286 0.9990 0.2579 11.00000 0.05 0.93
Q3 1 0.3552 0.2050 -0.0079 11.00000 0.05 0.88
Q4 1 0.2022 1.0237 0.2885 11.00000 0.05 0.81
Q5 1 0.5041 0.3605 -0.0509 11.00000 0.05 0.77
Q6 1 0.0873 0.9881 0.3061 11.00000 0.05 0.72
Q7 1 0.5179 0.0037 -0.0769 11.00000 0.05 0.69
Q8 1 0.2774 1.1820 0.2592 11.00000 0.05 0.60
Q9 1 0.1879 0.9929 0.1592 11.00000 0.05 0.58
Q10 1 0.4623 0.2419 -0.0263 11.00000 0.05 0.56
Q11 1 0.4165 0.1857 -0.0495 11.00000 0.05 0.56
Q12 1 0.4400 0.2139 -0.0360 11.00000 0.05 0.54
Q13 1 -0.0127 0.6751 0.1754 11.00000 0.05 0.53
Q14 1 0.0222 0.8971 0.2633 11.00000 0.05 0.52
Q15 1 0.3578 0.9969 0.2853 11.00000 0.05 0.51
Q16 1 0.5052 -0.1204 0.0104 11.00000 0.05 0.48
Q17 1 -0.3545 0.8587 0.2132 11.00000 0.05 0.48
Q18 1 0.1576 0.9680 0.4888 11.00000 0.05 0.48
Q19 1 0.3202 0.1202 0.0342 11.00000 0.05 0.47
Q20 1 0.1724 1.1431 0.4358 11.00000 0.05 0.46
;
_shelx_res_checksum 22968
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methylene chloride, hexane, toluene'