#------------------------------------------------------------------------------
#$Date: 2018-09-09 04:05:36 +0300 (Sun, 09 Sep 2018) $
#$Revision: 210600 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/10/36/7103689.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7103689
loop_
_publ_author_name
'Li, Yan'
'Huang, Jie-Sheng'
'Zhou, Zhong-Yuan'
'Che, Chi-Ming'
_publ_section_title
;
 Oxo-bridged metal carbene complexes. Synthesis, structure and
 reactivities of {[Os(Por)(CPh2)]2O} (Por = porphyrinato dianion)
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   12
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              1362
_journal_page_last               1363
_journal_paper_doi               10.1039/b300441d
_journal_year                    2003
_chemical_formula_sum            'C122 H92 N8 O Os2'
_chemical_formula_weight         2066.44
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.618(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.106(3)
_cell_length_b                   16.824(2)
_cell_length_c                   28.651(4)
_cell_measurement_reflns_used    10158
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     11075(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0903
_diffrn_reflns_av_sigmaI/netI    0.1350
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            37230
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         2.42
_exptl_absorpt_coefficient_mu    2.342
_exptl_absorpt_correction_T_max  0.6779
_exptl_absorpt_correction_T_min  0.4860
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS; Sheldrick 1996'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4160
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.924
_refine_diff_density_min         -2.845
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         12657
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1330
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0500P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1261
_refine_ls_wR_factor_ref         0.1489
_reflns_number_gt                6231
_reflns_number_total             12657
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b300441d.txt
_cod_data_source_block           complex_2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7103689
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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 0.418100(6) 0.390874(8) 0.717728(5) 0.03778(4) Uani 1 1 d . . .
O1 O 0.5000 0.39143(18) 0.7500 0.0404(10) Uani 1 2 d S . .
N1 N 0.42699(12) 0.28657(16) 0.68323(11) 0.0458(10) Uani 1 1 d . . .
N2 N 0.43400(12) 0.45658(16) 0.66273(10) 0.0433(9) Uani 1 1 d . . .
N3 N 0.40957(12) 0.49437(16) 0.75185(10) 0.0412(9) Uani 1 1 d . . .
N4 N 0.40688(11) 0.32572(17) 0.77468(11) 0.0452(9) Uani 1 1 d . . .
C1 C 0.41130(15) 0.1910(2) 0.74297(14) 0.0493(12) Uani 1 1 d . . .
C2 C 0.42141(16) 0.2111(2) 0.69924(15) 0.0506(13) Uani 1 1 d . . .
C3 C 0.42753(16) 0.1564(2) 0.66265(15) 0.0604(14) Uani 1 1 d . . .
H3 H 0.4254 0.1014 0.6642 0.072 Uiso 1 1 calc R . .
C4 C 0.43666(17) 0.1976(2) 0.62638(15) 0.0634(14) Uani 1 1 d . . .
H4 H 0.4433 0.1766 0.5985 0.076 Uiso 1 1 calc R . .
C5 C 0.43464(16) 0.2796(2) 0.63744(14) 0.0494(12) Uani 1 1 d . . .
C6 C 0.44006(15) 0.3443(2) 0.60815(14) 0.0490(12) Uani 1 1 d . . .
C7 C 0.44069(16) 0.4255(2) 0.61884(14) 0.0484(12) Uani 1 1 d . . .
C8 C 0.44376(17) 0.4911(2) 0.58772(14) 0.0581(14) Uani 1 1 d . . .
H8 H 0.4478 0.4874 0.5565 0.070 Uiso 1 1 calc R . .
C9 C 0.43976(17) 0.5584(2) 0.61123(14) 0.0580(13) Uani 1 1 d . . .
H9 H 0.4413 0.6096 0.5996 0.070 Uiso 1 1 calc R . .
C10 C 0.43253(16) 0.5371(2) 0.65875(13) 0.0473(12) Uani 1 1 d . . .
C11 C 0.42161(15) 0.5904(2) 0.69130(14) 0.0459(12) Uani 1 1 d . . .
C12 C 0.41060(15) 0.5708(2) 0.73369(13) 0.0447(11) Uani 1 1 d . . .
C13 C 0.39634(16) 0.6260(2) 0.76780(14) 0.0542(13) Uani 1 1 d . . .
H13 H 0.3945 0.6811 0.7649 0.065 Uiso 1 1 calc R . .
C14 C 0.38641(17) 0.5832(2) 0.80388(14) 0.0527(13) Uani 1 1 d . . .
H14 H 0.3756 0.6039 0.8299 0.063 Uiso 1 1 calc R . .
C15 C 0.39502(15) 0.5006(2) 0.79610(13) 0.0437(11) Uani 1 1 d . . .
C16 C 0.38615(15) 0.4373(2) 0.82373(13) 0.0440(12) Uani 1 1 d . . .
C17 C 0.39307(15) 0.3572(2) 0.81500(14) 0.0496(13) Uani 1 1 d . . .
C18 C 0.38555(18) 0.2920(2) 0.84547(16) 0.0668(15) Uani 1 1 d . . .
H18 H 0.3771 0.2962 0.8750 0.080 Uiso 1 1 calc R . .
C19 C 0.39297(18) 0.2244(2) 0.82327(15) 0.0660(15) Uani 1 1 d . . .
H19 H 0.3903 0.1733 0.8348 0.079 Uiso 1 1 calc R . .
C20 C 0.40598(15) 0.2438(2) 0.77794(14) 0.0481(12) Uani 1 1 d . . .
C21 C 0.40231(17) 0.1056(2) 0.75207(16) 0.0604(14) Uani 1 1 d . . .
C22 C 0.3545(2) 0.0654(3) 0.7270(2) 0.092(2) Uani 1 1 d . . .
H22 H 0.3267 0.0925 0.7025 0.110 Uiso 1 1 calc R . .
C23 C 0.3437(2) -0.0128(3) 0.7348(2) 0.099(2) Uani 1 1 d . . .
H23 H 0.3094 -0.0360 0.7156 0.119 Uiso 1 1 calc R . .
C24 C 0.3804(2) -0.0558(3) 0.7686(2) 0.092(2) Uani 1 1 d . . .
C25 C 0.4273(3) -0.0175(3) 0.7991(4) 0.227(5) Uani 1 1 d . . .
H25 H 0.4517 -0.0425 0.8266 0.272 Uiso 1 1 calc R . .
C26 C 0.4375(3) 0.0635(3) 0.7871(4) 0.242(5) Uani 1 1 d . . .
H26 H 0.4718 0.0876 0.8057 0.291 Uiso 1 1 calc R . .
C27 C 0.3703(3) -0.1424(3) 0.7789(2) 0.141(3) Uani 1 1 d . . .
H27A H 0.3540 -0.1454 0.8055 0.211 Uiso 1 1 calc R . .
H27B H 0.4067 -0.1704 0.7875 0.211 Uiso 1 1 calc R . .
H27C H 0.3439 -0.1659 0.7502 0.211 Uiso 1 1 calc R . .
C28 C 0.44339(17) 0.3252(2) 0.55765(14) 0.0575(14) Uani 1 1 d . . .
C29 C 0.49201(19) 0.3412(3) 0.54312(16) 0.0774(17) Uani 1 1 d . . .
H29 H 0.5244 0.3653 0.5647 0.093 Uiso 1 1 calc R . .
C30 C 0.4922(2) 0.3211(3) 0.49576(16) 0.0943(19) Uani 1 1 d . . .
H30 H 0.5247 0.3340 0.4863 0.113 Uiso 1 1 calc R . .
C31 C 0.4471(2) 0.2837(3) 0.46286(17) 0.094(2) Uani 1 1 d . . .
C32 C 0.4009(2) 0.2703(3) 0.47717(16) 0.095(2) Uani 1 1 d . . .
H32 H 0.3686 0.2473 0.4548 0.113 Uiso 1 1 calc R . .
C33 C 0.3971(2) 0.2882(3) 0.52320(16) 0.0771(18) Uani 1 1 d . . .
H33 H 0.3635 0.2754 0.5312 0.092 Uiso 1 1 calc R . .
C34 C 0.4496(3) 0.2633(4) 0.41343(17) 0.146(3) Uani 1 1 d . . .
H34A H 0.4474 0.3111 0.3946 0.220 Uiso 1 1 calc R . .
H34B H 0.4175 0.2292 0.3975 0.220 Uiso 1 1 calc R . .
H34C H 0.4855 0.2364 0.4160 0.220 Uiso 1 1 calc R . .
C35 C 0.41679(17) 0.6776(2) 0.67724(14) 0.0540(13) Uani 1 1 d . . .
C36 C 0.4643(2) 0.7238(2) 0.6816(2) 0.099(2) Uani 1 1 d . . .
H36 H 0.5014 0.7026 0.6947 0.119 Uiso 1 1 calc R . .
C37 C 0.4575(2) 0.8019(3) 0.6667(2) 0.118(2) Uani 1 1 d . . .
H37 H 0.4913 0.8313 0.6703 0.141 Uiso 1 1 calc R . .
C38 C 0.4079(2) 0.8385(3) 0.64785(17) 0.0799(17) Uani 1 1 d . . .
C39 C 0.3622(3) 0.7944(3) 0.6464(2) 0.129(3) Uani 1 1 d . . .
H39 H 0.3256 0.8180 0.6354 0.155 Uiso 1 1 calc R . .
C40 C 0.3652(2) 0.7144(3) 0.6603(2) 0.116(3) Uani 1 1 d . . .
H40 H 0.3311 0.6865 0.6577 0.139 Uiso 1 1 calc R . .
C41 C 0.4042(2) 0.9238(3) 0.6332(2) 0.131(2) Uani 1 1 d . . .
H41A H 0.4420 0.9478 0.6453 0.197 Uiso 1 1 calc R . .
H41B H 0.3775 0.9509 0.6468 0.197 Uiso 1 1 calc R . .
H41C H 0.3906 0.9278 0.5982 0.197 Uiso 1 1 calc R . .
C42 C 0.36331(15) 0.4570(2) 0.86581(13) 0.0496(12) Uani 1 1 d . . .
C43 C 0.30932(17) 0.4350(3) 0.86514(15) 0.0714(16) Uani 1 1 d . . .
H43 H 0.2861 0.4059 0.8388 0.086 Uiso 1 1 calc R . .
C44 C 0.28785(19) 0.4555(3) 0.90384(16) 0.0854(18) Uani 1 1 d . . .
H44 H 0.2506 0.4392 0.9027 0.102 Uiso 1 1 calc R . .
C45 C 0.31877(19) 0.4975(3) 0.94216(15) 0.0755(16) Uani 1 1 d . . .
C46 C 0.37335(19) 0.5183(3) 0.94336(15) 0.0746(17) Uani 1 1 d . . .
H46 H 0.3962 0.5464 0.9703 0.089 Uiso 1 1 calc R . .
C47 C 0.39668(18) 0.4996(2) 0.90627(14) 0.0614(14) Uani 1 1 d . . .
H47 H 0.4343 0.5154 0.9083 0.074 Uiso 1 1 calc R . .
C48 C 0.2928(2) 0.5192(4) 0.98303(17) 0.129(2) Uani 1 1 d . . .
H48A H 0.2511 0.5173 0.9706 0.193 Uiso 1 1 calc R . .
H48B H 0.3049 0.5719 0.9946 0.193 Uiso 1 1 calc R . .
H48C H 0.3062 0.4820 1.0095 0.193 Uiso 1 1 calc R . .
C49 C 0.33644(17) 0.3907(2) 0.68442(11) 0.0526(13) Uani 1 1 d . . .
C50 C 0.29985(15) 0.3146(2) 0.67155(15) 0.0569(14) Uani 1 1 d . . .
C51 C 0.29017(19) 0.2802(3) 0.62625(18) 0.0855(18) Uani 1 1 d . . .
H51 H 0.3065 0.3026 0.6037 0.103 Uiso 1 1 calc R . .
C52 C 0.2567(2) 0.2133(3) 0.61415(19) 0.094(2) Uani 1 1 d . . .
H52 H 0.2516 0.1892 0.5839 0.113 Uiso 1 1 calc R . .
C53 C 0.2304(2) 0.1814(3) 0.6463(2) 0.099(2) Uani 1 1 d . . .
H53 H 0.2067 0.1369 0.6375 0.119 Uiso 1 1 calc R . .
C54 C 0.23950(19) 0.2161(3) 0.69206(19) 0.0844(19) Uani 1 1 d . . .
H54 H 0.2228 0.1942 0.7144 0.101 Uiso 1 1 calc R . .
C55 C 0.27379(17) 0.2838(2) 0.70395(18) 0.0713(16) Uani 1 1 d . . .
H55 H 0.2791 0.3084 0.7341 0.086 Uiso 1 1 calc R . .
C56 C 0.29895(16) 0.4632(2) 0.66768(14) 0.0544(13) Uani 1 1 d . . .
C57 C 0.26961(19) 0.5011(3) 0.69707(17) 0.0783(18) Uani 1 1 d . . .
H57 H 0.2745 0.4814 0.7284 0.094 Uiso 1 1 calc R . .
C58 C 0.2349(2) 0.5642(3) 0.68199(19) 0.0913(19) Uani 1 1 d . . .
H58 H 0.2164 0.5875 0.7026 0.110 Uiso 1 1 calc R . .
C59 C 0.2270(2) 0.5943(3) 0.6361(2) 0.102(2) Uani 1 1 d . . .
H59 H 0.2030 0.6383 0.6258 0.122 Uiso 1 1 calc R . .
C60 C 0.2546(2) 0.5595(3) 0.6039(2) 0.108(2) Uani 1 1 d . . .
H60 H 0.2490 0.5797 0.5726 0.130 Uiso 1 1 calc R . .
C61 C 0.2915(2) 0.4921(3) 0.62123(17) 0.0865(18) Uani 1 1 d . . .
H61 H 0.3104 0.4679 0.6011 0.104 Uiso 1 1 calc R . .
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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -1.2165 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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 Os1 C49 179.02(11) . . ?
O1 Os1 N3 90.18(11) . . ?
C49 Os1 N3 90.16(14) . . ?
O1 Os1 N4 89.05(9) . . ?
C49 Os1 N4 91.86(13) . . ?
N3 Os1 N4 91.05(12) . . ?
O1 Os1 N2 87.89(9) . . ?
C49 Os1 N2 91.20(13) . . ?
N3 Os1 N2 88.71(12) . . ?
N4 Os1 N2 176.92(10) . . ?
O1 Os1 N1 89.66(11) . . ?
C49 Os1 N1 89.99(14) . . ?
N3 Os1 N1 179.78(13) . . ?
N4 Os1 N1 89.10(12) . . ?
N2 Os1 N1 91.13(12) . . ?
Os1 O1 Os1 179.44(18) 2_656 . ?
C2 N1 C5 107.1(3) . . ?
C2 N1 Os1 126.5(3) . . ?
C5 N1 Os1 126.2(2) . . ?
C10 N2 C7 107.5(3) . . ?
C10 N2 Os1 126.5(3) . . ?
C7 N2 Os1 125.5(2) . . ?
C12 N3 C15 107.7(3) . . ?
C12 N3 Os1 126.5(3) . . ?
C15 N3 Os1 125.5(2) . . ?
C20 N4 C17 108.0(3) . . ?
C20 N4 Os1 126.6(3) . . ?
C17 N4 Os1 125.2(2) . . ?
C20 C1 C2 125.5(3) . . ?
C20 C1 C21 116.5(4) . . ?
C2 C1 C21 117.9(4) . . ?
N1 C2 C1 126.1(3) . . ?
N1 C2 C3 107.9(4) . . ?
C1 C2 C3 126.0(3) . . ?
C4 C3 C2 108.5(4) . . ?
C4 C3 H3 125.8 . . ?
C2 C3 H3 125.8 . . ?
C3 C4 C5 108.0(4) . . ?
C3 C4 H4 126.0 . . ?
C5 C4 H4 126.0 . . ?
N1 C5 C6 124.4(3) . . ?
N1 C5 C4 108.5(3) . . ?
C6 C5 C4 127.1(4) . . ?
C7 C6 C5 128.5(4) . . ?
C7 C6 C28 114.7(4) . . ?
C5 C6 C28 116.8(3) . . ?
C6 C7 N2 123.9(4) . . ?
C6 C7 C8 127.9(4) . . ?
N2 C7 C8 108.0(3) . . ?
C9 C8 C7 108.2(4) . . ?
C9 C8 H8 125.9 . . ?
C7 C8 H8 125.9 . . ?
C8 C9 C10 108.0(4) . . ?
C8 C9 H9 126.0 . . ?
C10 C9 H9 126.0 . . ?
N2 C10 C11 126.8(4) . . ?
N2 C10 C9 108.3(3) . . ?
C11 C10 C9 124.8(3) . . ?
C12 C11 C10 125.1(3) . . ?
C12 C11 C35 116.9(3) . . ?
C10 C11 C35 117.8(4) . . ?
C11 C12 N3 126.1(3) . . ?
C11 C12 C13 126.2(3) . . ?
N3 C12 C13 107.6(3) . . ?
C14 C13 C12 107.9(3) . . ?
C14 C13 H13 126.1 . . ?
C12 C13 H13 126.1 . . ?
C13 C14 C15 109.5(4) . . ?
C13 C14 H14 125.3 . . ?
C15 C14 H14 125.3 . . ?
C16 C15 N3 125.3(3) . . ?
C16 C15 C14 127.2(4) . . ?
N3 C15 C14 107.3(3) . . ?
C15 C16 C17 126.6(4) . . ?
C15 C16 C42 116.5(3) . . ?
C17 C16 C42 116.8(3) . . ?
C16 C17 N4 126.0(4) . . ?
C16 C17 C18 125.6(4) . . ?
N4 C17 C18 108.4(3) . . ?
C19 C18 C17 107.3(4) . . ?
C19 C18 H18 126.3 . . ?
C17 C18 H18 126.3 . . ?
C18 C19 C20 109.1(4) . . ?
C18 C19 H19 125.5 . . ?
C20 C19 H19 125.5 . . ?
C1 C20 N4 126.1(4) . . ?
C1 C20 C19 126.6(3) . . ?
N4 C20 C19 107.1(3) . . ?
C26 C21 C22 113.0(4) . . ?
C26 C21 C1 124.2(4) . . ?
C22 C21 C1 122.7(4) . . ?
C21 C22 C23 124.8(4) . . ?
C21 C22 H22 117.6 . . ?
C23 C22 H22 117.6 . . ?
C24 C23 C22 122.0(4) . . ?
C24 C23 H23 119.0 . . ?
C22 C23 H23 119.0 . . ?
C23 C24 C25 117.0(5) . . ?
C23 C24 C27 124.0(4) . . ?
C25 C24 C27 118.7(5) . . ?
C24 C25 C26 117.6(6) . . ?
C24 C25 H25 121.2 . . ?
C26 C25 H25 121.2 . . ?
C21 C26 C25 125.1(6) . . ?
C21 C26 H26 117.5 . . ?
C25 C26 H26 117.5 . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 C28 C33 116.4(4) . . ?
C29 C28 C6 122.9(3) . . ?
C33 C28 C6 120.7(4) . . ?
C28 C29 C30 119.7(4) . . ?
C28 C29 H29 120.2 . . ?
C30 C29 H29 120.2 . . ?
C31 C30 C29 123.3(5) . . ?
C31 C30 H30 118.4 . . ?
C29 C30 H30 118.4 . . ?
C32 C31 C30 115.9(5) . . ?
C32 C31 C34 122.9(5) . . ?
C30 C31 C34 121.1(5) . . ?
C31 C32 C33 124.5(5) . . ?
C31 C32 H32 117.7 . . ?
C33 C32 H32 117.7 . . ?
C32 C33 C28 120.2(5) . . ?
C32 C33 H33 119.9 . . ?
C28 C33 H33 119.9 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C40 C35 C36 115.6(4) . . ?
C40 C35 C11 122.1(4) . . ?
C36 C35 C11 122.3(3) . . ?
C35 C36 C37 120.0(4) . . ?
C35 C36 H36 120.0 . . ?
C37 C36 H36 120.0 . . ?
C38 C37 C36 125.9(5) . . ?
C38 C37 H37 117.1 . . ?
C36 C37 H37 117.1 . . ?
C37 C38 C39 113.6(4) . . ?
C37 C38 C41 122.7(5) . . ?
C39 C38 C41 123.6(4) . . ?
C38 C39 C40 124.1(5) . . ?
C38 C39 H39 118.0 . . ?
C40 C39 H39 118.0 . . ?
C35 C40 C39 120.7(5) . . ?
C35 C40 H40 119.7 . . ?
C39 C40 H40 119.7 . . ?
C38 C41 H41A 109.5 . . ?
C38 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C38 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C43 C42 C47 117.7(4) . . ?
C43 C42 C16 120.9(3) . . ?
C47 C42 C16 121.3(4) . . ?
C42 C43 C44 120.5(4) . . ?
C42 C43 H43 119.8 . . ?
C44 C43 H43 119.8 . . ?
C45 C44 C43 122.4(4) . . ?
C45 C44 H44 118.8 . . ?
C43 C44 H44 118.8 . . ?
C44 C45 C46 117.2(4) . . ?
C44 C45 C48 120.2(4) . . ?
C46 C45 C48 122.6(4) . . ?
C45 C46 C47 122.8(4) . . ?
C45 C46 H46 118.6 . . ?
C47 C46 H46 118.6 . . ?
C46 C47 C42 119.4(4) . . ?
C46 C47 H47 120.3 . . ?
C42 C47 H47 120.3 . . ?
C45 C48 H48A 109.5 . . ?
C45 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C45 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C56 C49 C50 110.7(3) . . ?
C56 C49 Os1 125.8(3) . . ?
C50 C49 Os1 123.5(3) . . ?
C55 C50 C51 119.9(4) . . ?
C55 C50 C49 120.0(4) . . ?
C51 C50 C49 119.9(4) . . ?
C52 C51 C50 120.3(5) . . ?
C52 C51 H51 119.9 . . ?
C50 C51 H51 119.9 . . ?
C51 C52 C53 120.5(5) . . ?
C51 C52 H52 119.7 . . ?
C53 C52 H52 119.7 . . ?
C52 C53 C54 119.6(5) . . ?
C52 C53 H53 120.2 . . ?
C54 C53 H53 120.2 . . ?
C55 C54 C53 119.2(5) . . ?
C55 C54 H54 120.4 . . ?
C53 C54 H54 120.4 . . ?
C50 C55 C54 120.3(5) . . ?
C50 C55 H55 119.8 . . ?
C54 C55 H55 119.8 . . ?
C61 C56 C57 118.5(4) . . ?
C61 C56 C49 118.9(4) . . ?
C57 C56 C49 122.6(4) . . ?
C58 C57 C56 123.0(5) . . ?
C58 C57 H57 118.5 . . ?
C56 C57 H57 118.5 . . ?
C57 C58 C59 119.7(5) . . ?
C57 C58 H58 120.2 . . ?
C59 C58 H58 120.2 . . ?
C58 C59 C60 121.1(5) . . ?
C58 C59 H59 119.4 . . ?
C60 C59 H59 119.4 . . ?
C59 C60 C61 117.7(5) . . ?
C59 C60 H60 121.1 . . ?
C61 C60 H60 121.1 . . ?
C56 C61 C60 120.0(5) . . ?
C56 C61 H61 120.0 . . ?
C60 C61 H61 120.0 . . ?
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 O1 1.9099(3) . ?
Os1 C49 1.910(4) . ?
Os1 N3 2.038(3) . ?
Os1 N4 2.050(3) . ?
Os1 N2 2.054(3) . ?
Os1 N1 2.057(3) . ?
O1 Os1 1.9099(3) 2_656 ?
N1 C2 1.370(5) . ?
N1 C5 1.384(5) . ?
N2 C10 1.359(4) . ?
N2 C7 1.415(5) . ?
N3 C12 1.390(4) . ?
N3 C15 1.418(5) . ?
N4 C20 1.382(4) . ?
N4 C17 1.400(5) . ?
C1 C20 1.374(5) . ?
C1 C2 1.389(6) . ?
C1 C21 1.488(5) . ?
C2 C3 1.436(6) . ?
C3 C4 1.322(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.420(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.403(5) . ?
C6 C7 1.400(5) . ?
C6 C28 1.508(6) . ?
C7 C8 1.434(5) . ?
C8 C9 1.335(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.468(6) . ?
C9 H9 0.9300 . ?
C10 C11 1.376(5) . ?
C11 C12 1.360(6) . ?
C11 C35 1.515(5) . ?
C12 C13 1.463(5) . ?
C13 C14 1.340(6) . ?
C13 H13 0.9300 . ?
C14 C15 1.431(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.382(5) . ?
C16 C17 1.389(5) . ?
C16 C42 1.506(6) . ?
C17 C18 1.447(6) . ?
C18 C19 1.342(6) . ?
C18 H18 0.9300 . ?
C19 C20 1.462(6) . ?
C19 H19 0.9300 . ?
C21 C26 1.309(8) . ?
C21 C22 1.342(6) . ?
C22 C23 1.373(6) . ?
C22 H22 0.9300 . ?
C23 C24 1.315(6) . ?
C23 H23 0.9300 . ?
C24 C25 1.363(8) . ?
C24 C27 1.519(7) . ?
C25 C26 1.444(9) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 C29 1.384(6) . ?
C28 C33 1.393(5) . ?
C29 C30 1.400(6) . ?
C29 H29 0.9300 . ?
C30 C31 1.358(6) . ?
C30 H30 0.9300 . ?
C31 C32 1.317(8) . ?
C31 C34 1.476(7) . ?
C32 C33 1.383(7) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 C40 1.342(6) . ?
C35 C36 1.358(6) . ?
C36 C37 1.377(6) . ?
C36 H36 0.9300 . ?
C37 C38 1.308(6) . ?
C37 H37 0.9300 . ?
C38 C39 1.320(7) . ?
C38 C41 1.491(6) . ?
C39 C40 1.399(7) . ?
C39 H39 0.9300 . ?
C40 H40 0.9300 . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 C43 1.348(5) . ?
C42 C47 1.394(5) . ?
C43 C44 1.402(6) . ?
C43 H43 0.9300 . ?
C44 C45 1.329(6) . ?
C44 H44 0.9300 . ?
C45 C46 1.352(6) . ?
C45 C48 1.529(7) . ?
C46 C47 1.380(6) . ?
C46 H46 0.9300 . ?
C47 H47 0.9300 . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C49 C56 1.508(5) . ?
C49 C50 1.534(5) . ?
C50 C55 1.370(6) . ?
C50 C51 1.375(6) . ?
C51 C52 1.367(6) . ?
C51 H51 0.9300 . ?
C52 C53 1.376(8) . ?
C52 H52 0.9300 . ?
C53 C54 1.390(7) . ?
C53 H53 0.9300 . ?
C54 C55 1.388(6) . ?
C54 H54 0.9300 . ?
C55 H55 0.9300 . ?
C56 C61 1.377(6) . ?
C56 C57 1.406(6) . ?
C57 C58 1.340(6) . ?
C57 H57 0.9300 . ?
C58 C59 1.368(8) . ?
C58 H58 0.9300 . ?
C59 C60 1.416(8) . ?
C59 H59 0.9300 . ?
C60 C61 1.434(7) . ?
C60 H60 0.9300 . ?
C61 H61 0.9300 . ?
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
C49 Os1 O1 Os1 -101(9) . . . 2_656 ?
N3 Os1 O1 Os1 148.7(2) . . . 2_656 ?
N4 Os1 O1 Os1 57.7(2) . . . 2_656 ?
N2 Os1 O1 Os1 -122.6(2) . . . 2_656 ?
N1 Os1 O1 Os1 -31.4(2) . . . 2_656 ?
O1 Os1 N1 C2 92.7(3) . . . . ?
C49 Os1 N1 C2 -88.2(3) . . . . ?
N3 Os1 N1 C2 136(43) . . . . ?
N4 Os1 N1 C2 3.6(3) . . . . ?
N2 Os1 N1 C2 -179.4(3) . . . . ?
O1 Os1 N1 C5 -93.4(3) . . . . ?
C49 Os1 N1 C5 85.7(3) . . . . ?
N3 Os1 N1 C5 -50(43) . . . . ?
N4 Os1 N1 C5 177.5(3) . . . . ?
N2 Os1 N1 C5 -5.5(3) . . . . ?
O1 Os1 N2 C10 -93.9(3) . . . . ?
C49 Os1 N2 C10 86.5(3) . . . . ?
N3 Os1 N2 C10 -3.7(3) . . . . ?
N4 Os1 N2 C10 -89(2) . . . . ?
N1 Os1 N2 C10 176.5(3) . . . . ?
O1 Os1 N2 C7 95.2(3) . . . . ?
C49 Os1 N2 C7 -84.4(3) . . . . ?
N3 Os1 N2 C7 -174.5(3) . . . . ?
N4 Os1 N2 C7 100(2) . . . . ?
N1 Os1 N2 C7 5.6(3) . . . . ?
O1 Os1 N3 C12 93.0(3) . . . . ?
C49 Os1 N3 C12 -86.1(3) . . . . ?
N4 Os1 N3 C12 -178.0(3) . . . . ?
N2 Os1 N3 C12 5.1(3) . . . . ?
N1 Os1 N3 C12 49(43) . . . . ?
O1 Os1 N3 C15 -94.5(2) . . . . ?
C49 Os1 N3 C15 86.4(3) . . . . ?
N4 Os1 N3 C15 -5.5(3) . . . . ?
N2 Os1 N3 C15 177.6(3) . . . . ?
N1 Os1 N3 C15 -138(43) . . . . ?
O1 Os1 N4 C20 -91.2(3) . . . . ?
C49 Os1 N4 C20 88.4(3) . . . . ?
N3 Os1 N4 C20 178.6(3) . . . . ?
N2 Os1 N4 C20 -96(2) . . . . ?
N1 Os1 N4 C20 -1.6(3) . . . . ?
O1 Os1 N4 C17 95.4(3) . . . . ?
C49 Os1 N4 C17 -84.9(3) . . . . ?
N3 Os1 N4 C17 5.3(3) . . . . ?
N2 Os1 N4 C17 91(2) . . . . ?
N1 Os1 N4 C17 -174.9(3) . . . . ?
C5 N1 C2 C1 -178.0(3) . . . . ?
Os1 N1 C2 C1 -3.1(5) . . . . ?
C5 N1 C2 C3 1.7(4) . . . . ?
Os1 N1 C2 C3 176.5(2) . . . . ?
C20 C1 C2 N1 -1.0(6) . . . . ?
C21 C1 C2 N1 175.7(3) . . . . ?
C20 C1 C2 C3 179.4(4) . . . . ?
C21 C1 C2 C3 -4.0(5) . . . . ?
N1 C2 C3 C4 0.3(4) . . . . ?
C1 C2 C3 C4 179.9(4) . . . . ?
C2 C3 C4 C5 -2.1(4) . . . . ?
C2 N1 C5 C6 177.8(3) . . . . ?
Os1 N1 C5 C6 2.9(5) . . . . ?
C2 N1 C5 C4 -2.9(4) . . . . ?
Os1 N1 C5 C4 -177.8(2) . . . . ?
C3 C4 C5 N1 3.2(4) . . . . ?
C3 C4 C5 C6 -177.6(4) . . . . ?
N1 C5 C6 C7 2.1(6) . . . . ?
C4 C5 C6 C7 -177.1(4) . . . . ?
N1 C5 C6 C28 -175.3(3) . . . . ?
C4 C5 C6 C28 5.5(5) . . . . ?
C5 C6 C7 N2 -1.9(6) . . . . ?
C28 C6 C7 N2 175.6(3) . . . . ?
C5 C6 C7 C8 -177.1(4) . . . . ?
C28 C6 C7 C8 0.3(5) . . . . ?
C10 N2 C7 C6 -175.5(3) . . . . ?
Os1 N2 C7 C6 -3.2(5) . . . . ?
C10 N2 C7 C8 0.5(4) . . . . ?
Os1 N2 C7 C8 172.8(2) . . . . ?
C6 C7 C8 C9 176.4(4) . . . . ?
N2 C7 C8 C9 0.5(4) . . . . ?
C7 C8 C9 C10 -1.3(4) . . . . ?
C7 N2 C10 C11 174.0(3) . . . . ?
Os1 N2 C10 C11 1.8(5) . . . . ?
C7 N2 C10 C9 -1.2(4) . . . . ?
Os1 N2 C10 C9 -173.4(2) . . . . ?
C8 C9 C10 N2 1.6(4) . . . . ?
C8 C9 C10 C11 -173.8(4) . . . . ?
N2 C10 C11 C12 0.4(6) . . . . ?
C9 C10 C11 C12 174.9(3) . . . . ?
N2 C10 C11 C35 -174.6(3) . . . . ?
C9 C10 C11 C35 -0.1(5) . . . . ?
C10 C11 C12 N3 1.3(6) . . . . ?
C35 C11 C12 N3 176.4(3) . . . . ?
C10 C11 C12 C13 -177.1(3) . . . . ?
C35 C11 C12 C13 -2.1(5) . . . . ?
C15 N3 C12 C11 -178.6(3) . . . . ?
Os1 N3 C12 C11 -5.0(5) . . . . ?
C15 N3 C12 C13 0.1(4) . . . . ?
Os1 N3 C12 C13 173.7(2) . . . . ?
C11 C12 C13 C14 177.6(3) . . . . ?
N3 C12 C13 C14 -1.0(4) . . . . ?
C12 C13 C14 C15 1.6(4) . . . . ?
C12 N3 C15 C16 175.8(3) . . . . ?
Os1 N3 C15 C16 2.1(5) . . . . ?
C12 N3 C15 C14 0.8(4) . . . . ?
Os1 N3 C15 C14 -172.9(2) . . . . ?
C13 C14 C15 C16 -176.4(3) . . . . ?
C13 C14 C15 N3 -1.5(4) . . . . ?
N3 C15 C16 C17 4.0(6) . . . . ?
C14 C15 C16 C17 178.0(3) . . . . ?
N3 C15 C16 C42 -172.1(3) . . . . ?
C14 C15 C16 C42 1.9(5) . . . . ?
C15 C16 C17 N4 -4.2(6) . . . . ?
C42 C16 C17 N4 171.9(3) . . . . ?
C15 C16 C17 C18 177.6(3) . . . . ?
C42 C16 C17 C18 -6.3(5) . . . . ?
C20 N4 C17 C16 -176.1(3) . . . . ?
Os1 N4 C17 C16 -1.7(5) . . . . ?
C20 N4 C17 C18 2.3(4) . . . . ?
Os1 N4 C17 C18 176.7(2) . . . . ?
C16 C17 C18 C19 176.7(4) . . . . ?
N4 C17 C18 C19 -1.7(4) . . . . ?
C17 C18 C19 C20 0.5(4) . . . . ?
C2 C1 C20 N4 3.4(6) . . . . ?
C21 C1 C20 N4 -173.3(3) . . . . ?
C2 C1 C20 C19 177.3(4) . . . . ?
C21 C1 C20 C19 0.6(5) . . . . ?
C17 N4 C20 C1 172.9(3) . . . . ?
Os1 N4 C20 C1 -1.4(5) . . . . ?
C17 N4 C20 C19 -2.0(4) . . . . ?
Os1 N4 C20 C19 -176.3(2) . . . . ?
C18 C19 C20 C1 -173.9(4) . . . . ?
C18 C19 C20 N4 1.0(4) . . . . ?
C20 C1 C21 C26 -68.0(8) . . . . ?
C2 C1 C21 C26 115.1(7) . . . . ?
C20 C1 C21 C22 107.1(5) . . . . ?
C2 C1 C21 C22 -69.8(6) . . . . ?
C26 C21 C22 C23 -2.9(9) . . . . ?
C1 C21 C22 C23 -178.4(5) . . . . ?
C21 C22 C23 C24 0.2(10) . . . . ?
C22 C23 C24 C25 6.3(10) . . . . ?
C22 C23 C24 C27 179.7(6) . . . . ?
C23 C24 C25 C26 -9.4(12) . . . . ?
C27 C24 C25 C26 176.9(7) . . . . ?
C22 C21 C26 C25 -0.8(13) . . . . ?
C1 C21 C26 C25 174.7(8) . . . . ?
C24 C25 C26 C21 7.1(15) . . . . ?
C7 C6 C28 C29 66.4(5) . . . . ?
C5 C6 C28 C29 -115.9(4) . . . . ?
C7 C6 C28 C33 -115.1(4) . . . . ?
C5 C6 C28 C33 62.6(5) . . . . ?
C33 C28 C29 C30 0.8(6) . . . . ?
C6 C28 C29 C30 179.3(4) . . . . ?
C28 C29 C30 C31 -2.1(8) . . . . ?
C29 C30 C31 C32 3.3(8) . . . . ?
C29 C30 C31 C34 -179.6(5) . . . . ?
C30 C31 C32 C33 -3.3(8) . . . . ?
C34 C31 C32 C33 179.6(5) . . . . ?
C31 C32 C33 C28 2.2(8) . . . . ?
C29 C28 C33 C32 -0.8(6) . . . . ?
C6 C28 C33 C32 -179.4(4) . . . . ?
C12 C11 C35 C40 -73.5(5) . . . . ?
C10 C11 C35 C40 101.9(5) . . . . ?
C12 C11 C35 C36 105.5(5) . . . . ?
C10 C11 C35 C36 -79.1(5) . . . . ?
C40 C35 C36 C37 -3.3(8) . . . . ?
C11 C35 C36 C37 177.7(5) . . . . ?
C35 C36 C37 C38 0.1(10) . . . . ?
C36 C37 C38 C39 3.6(10) . . . . ?
C36 C37 C38 C41 179.0(6) . . . . ?
C37 C38 C39 C40 -4.3(10) . . . . ?
C41 C38 C39 C40 -179.6(6) . . . . ?
C36 C35 C40 C39 2.6(8) . . . . ?
C11 C35 C40 C39 -178.3(5) . . . . ?
C38 C39 C40 C35 1.3(10) . . . . ?
C15 C16 C42 C43 112.2(4) . . . . ?
C17 C16 C42 C43 -64.3(5) . . . . ?
C15 C16 C42 C47 -66.6(5) . . . . ?
C17 C16 C42 C47 116.9(4) . . . . ?
C47 C42 C43 C44 0.7(6) . . . . ?
C16 C42 C43 C44 -178.2(4) . . . . ?
C42 C43 C44 C45 0.6(7) . . . . ?
C43 C44 C45 C46 -1.9(7) . . . . ?
C43 C44 C45 C48 179.2(5) . . . . ?
C44 C45 C46 C47 1.9(7) . . . . ?
C48 C45 C46 C47 -179.2(4) . . . . ?
C45 C46 C47 C42 -0.6(7) . . . . ?
C43 C42 C47 C46 -0.7(6) . . . . ?
C16 C42 C47 C46 178.2(4) . . . . ?
O1 Os1 C49 C56 -78(9) . . . . ?
N3 Os1 C49 C56 33.2(3) . . . . ?
N4 Os1 C49 C56 124.2(3) . . . . ?
N2 Os1 C49 C56 -55.5(3) . . . . ?
N1 Os1 C49 C56 -146.7(3) . . . . ?
O1 Os1 C49 C50 103(9) . . . . ?
N3 Os1 C49 C50 -146.1(3) . . . . ?
N4 Os1 C49 C50 -55.1(3) . . . . ?
N2 Os1 C49 C50 125.2(3) . . . . ?
N1 Os1 C49 C50 34.0(3) . . . . ?
C56 C49 C50 C55 -89.4(4) . . . . ?
Os1 C49 C50 C55 90.0(4) . . . . ?
C56 C49 C50 C51 86.5(5) . . . . ?
Os1 C49 C50 C51 -94.1(4) . . . . ?
C55 C50 C51 C52 -2.9(6) . . . . ?
C49 C50 C51 C52 -178.7(4) . . . . ?
C50 C51 C52 C53 2.6(7) . . . . ?
C51 C52 C53 C54 -2.0(7) . . . . ?
C52 C53 C54 C55 1.7(7) . . . . ?
C51 C50 C55 C54 2.6(6) . . . . ?
C49 C50 C55 C54 178.5(4) . . . . ?
C53 C54 C55 C50 -2.0(6) . . . . ?
C50 C49 C56 C61 -89.6(5) . . . . ?
Os1 C49 C56 C61 91.0(4) . . . . ?
C50 C49 C56 C57 88.2(4) . . . . ?
Os1 C49 C56 C57 -91.2(5) . . . . ?
C61 C56 C57 C58 -0.3(7) . . . . ?
C49 C56 C57 C58 -178.1(4) . . . . ?
C56 C57 C58 C59 0.1(7) . . . . ?
C57 C58 C59 C60 0.3(8) . . . . ?
C58 C59 C60 C61 -0.4(7) . . . . ?
C57 C56 C61 C60 0.2(6) . . . . ?
C49 C56 C61 C60 178.1(4) . . . . ?
C59 C60 C61 C56 0.1(7) . . . . ?
