#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/36/4303626.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_4303626
loop_
_publ_author_name
'Gabriel E. Büchel'
'Iryna N. Stepanenko'
'Michaela Hejl'
'Michael A. Jakupec'
'Vladimir B. Arion'
'Bernhard K. Keppler'
_publ_section_title
;
[OsIVCl5(Hazole)]- Complexes: Synthesis, Structure, Spectroscopic
Properties, and Antiproliferative Activity
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10737
_journal_page_last               10747
_journal_paper_doi               10.1021/ic901671j
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C16 H36 N, C2 H3 Cl5 N3 Os, C2 H6 O'
_chemical_formula_sum            'C20 H45 Cl5 N4 O Os'
_chemical_formula_weight         725.05
_chemical_name_systematic
; 
tetrabutylammonium-pentachloridotriazoleosmate(IV) ethanol solvate 
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.195(2)
_cell_angle_beta                 103.674(2)
_cell_angle_gamma                90.0200(10)
_cell_formula_units_Z            2
_cell_length_a                   9.6679(3)
_cell_length_b                   10.4061(3)
_cell_length_c                   15.1487(6)
_cell_measurement_reflns_used    1719
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.83
_cell_measurement_theta_min      2.35
_cell_volume                     1464.80(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0367
_diffrn_reflns_av_sigmaI/netI    0.0416
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            42583
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.59
_exptl_absorpt_coefficient_mu    4.828
_exptl_absorpt_correction_T_max  0.9096
_exptl_absorpt_correction_T_min  0.3253
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.706
_refine_diff_density_min         -1.559
_refine_diff_density_rms         0.125
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.021(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         13386
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0264
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0385P)²+0.0962P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0659
_refine_ls_wR_factor_ref         0.0669
_reflns_number_gt                12810
_reflns_number_total             13386
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901671j_si_002_3.cif
_cod_data_source_block           gabu015
_cod_original_cell_volume        1464.80(8)
_cod_original_sg_symbol_Hall     P1
_cod_database_code               4303626
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
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 0.037574(12) 0.664550(11) 0.124923(10) 0.01115(5) Uani 1 1 d . . .
Cl1 Cl 0.19301(12) 0.49437(10) 0.13262(9) 0.0203(2) Uani 1 1 d . . .
Cl2 Cl -0.05438(11) 0.60039(10) 0.24071(8) 0.0164(2) Uani 1 1 d . . .
Cl3 Cl -0.10950(11) 0.84336(10) 0.12097(9) 0.0181(2) Uani 1 1 d . . .
Cl4 Cl 0.13597(11) 0.73655(10) 0.01423(8) 0.0173(2) Uani 1 1 d . . .
Cl5 Cl -0.13806(12) 0.53699(11) 0.01607(8) 0.0205(2) Uani 1 1 d . . .
N1 N 0.1924(4) 0.7764(3) 0.2261(3) 0.0121(7) Uani 1 1 d . . .
N2 N 0.1607(4) 0.8487(4) 0.3018(3) 0.0196(9) Uani 1 1 d . . .
N3 N 0.3904(4) 0.8603(4) 0.3141(3) 0.0198(9) Uani 1 1 d . . .
H3 H 0.4814 0.8821 0.3361 0.024 Uiso 1 1 calc R . .
C1 C 0.2822(5) 0.8968(5) 0.3531(4) 0.0257(12) Uani 1 1 d . . .
H1 H 0.2933 0.9508 0.4106 0.031 Uiso 1 1 calc R . .
C2 C 0.3315(5) 0.7846(4) 0.2355(3) 0.0137(9) Uani 1 1 d . . .
H2 H 0.3816 0.7431 0.1931 0.016 Uiso 1 1 calc R . .
N7 N 0.6355(4) 0.2415(3) 0.1756(3) 0.0136(8) Uani 1 1 d . . .
C3 C 0.6057(5) 0.3786(4) 0.2156(3) 0.0163(9) Uani 1 1 d . . .
H3A H 0.5250 0.4110 0.1720 0.020 Uiso 1 1 calc R . .
H3B H 0.6901 0.4355 0.2207 0.020 Uiso 1 1 calc R . .
C4 C 0.5706(5) 0.3916(5) 0.3098(4) 0.0193(10) Uani 1 1 d . . .
H4A H 0.4799 0.3436 0.3045 0.023 Uiso 1 1 calc R . .
H4B H 0.6466 0.3529 0.3531 0.023 Uiso 1 1 calc R . .
C5 C 0.5577(6) 0.5332(5) 0.3469(4) 0.0274(12) Uani 1 1 d . . .
H5A H 0.6512 0.5792 0.3577 0.033 Uiso 1 1 calc R . .
H5B H 0.4886 0.5740 0.3007 0.033 Uiso 1 1 calc R . .
C6 C 0.5093(6) 0.5479(6) 0.4354(5) 0.0363(14) Uani 1 1 d . . .
H6A H 0.5007 0.6403 0.4569 0.054 Uiso 1 1 calc R . .
H6B H 0.5792 0.5103 0.4820 0.054 Uiso 1 1 calc R . .
H6C H 0.4166 0.5027 0.4249 0.054 Uiso 1 1 calc R . .
C7 C 0.5124(4) 0.1462(4) 0.1709(3) 0.0147(9) Uani 1 1 d . . .
H7A H 0.5366 0.0587 0.1449 0.018 Uiso 1 1 calc R . .
H7B H 0.5036 0.1420 0.2342 0.018 Uiso 1 1 calc R . .
C8 C 0.3689(5) 0.1797(4) 0.1141(4) 0.0188(10) Uani 1 1 d . . .
H8A H 0.3741 0.1782 0.0495 0.023 Uiso 1 1 calc R . .
H8B H 0.3448 0.2684 0.1377 0.023 Uiso 1 1 calc R . .
C9 C 0.2534(5) 0.0830(4) 0.1184(4) 0.0202(10) Uani 1 1 d . . .
H9A H 0.2750 -0.0048 0.0914 0.024 Uiso 1 1 calc R . .
H9B H 0.2531 0.0804 0.1835 0.024 Uiso 1 1 calc R . .
C10 C 0.1071(5) 0.1189(5) 0.0672(4) 0.0239(11) Uani 1 1 d . . .
H10A H 0.0356 0.0549 0.0716 0.036 Uiso 1 1 calc R . .
H10B H 0.1066 0.1198 0.0025 0.036 Uiso 1 1 calc R . .
H10C H 0.0848 0.2052 0.0945 0.036 Uiso 1 1 calc R . .
C11 C 0.6562(5) 0.2507(4) 0.0796(3) 0.0173(9) Uani 1 1 d . . .
H11A H 0.5705 0.2894 0.0449 0.021 Uiso 1 1 calc R . .
H11B H 0.7379 0.3115 0.0862 0.021 Uiso 1 1 calc R . .
C12 C 0.6819(5) 0.1250(5) 0.0227(4) 0.0215(10) Uani 1 1 d . . .
H12A H 0.7660 0.0835 0.0567 0.026 Uiso 1 1 calc R . .
H12B H 0.5984 0.0646 0.0117 0.026 Uiso 1 1 calc R . .
C13 C 0.7066(6) 0.1502(5) -0.0685(4) 0.0286(12) Uani 1 1 d . . .
H13A H 0.7898 0.2111 -0.0570 0.034 Uiso 1 1 calc R . .
H13B H 0.6224 0.1923 -0.1020 0.034 Uiso 1 1 calc R . .
C14 C 0.7329(7) 0.0262(6) -0.1281(5) 0.0368(14) Uani 1 1 d . . .
H14A H 0.7498 0.0477 -0.1857 0.055 Uiso 1 1 calc R . .
H14B H 0.6494 -0.0331 -0.1416 0.055 Uiso 1 1 calc R . .
H14C H 0.8165 -0.0156 -0.0954 0.055 Uiso 1 1 calc R . .
C15 C 0.7669(4) 0.1896(4) 0.2358(4) 0.0153(9) Uani 1 1 d . . .
H15A H 0.7445 0.1760 0.2943 0.018 Uiso 1 1 calc R . .
H15B H 0.7869 0.1038 0.2047 0.018 Uiso 1 1 calc R . .
C16 C 0.9001(4) 0.2755(4) 0.2574(3) 0.0166(9) Uani 1 1 d . . .
H16A H 0.8870 0.3565 0.2972 0.020 Uiso 1 1 calc R . .
H16B H 0.9170 0.2993 0.1998 0.020 Uiso 1 1 calc R . .
C17 C 1.0290(5) 0.2068(5) 0.3059(4) 0.0193(10) Uani 1 1 d . . .
H17A H 1.0124 0.1838 0.3639 0.023 Uiso 1 1 calc R . .
H17B H 1.0414 0.1253 0.2665 0.023 Uiso 1 1 calc R . .
C18 C 1.1635(5) 0.2918(6) 0.3271(4) 0.0242(11) Uani 1 1 d . . .
H18A H 1.2442 0.2453 0.3585 0.036 Uiso 1 1 calc R . .
H18B H 1.1519 0.3721 0.3668 0.036 Uiso 1 1 calc R . .
H18C H 1.1814 0.3131 0.2697 0.036 Uiso 1 1 calc R . .
Os2 Os 0.703533(13) 0.098363(12) 0.545220(10) 0.01191(5) Uani 1 1 d . . .
Cl6 Cl 0.83329(11) 0.27084(10) 0.51617(8) 0.0171(2) Uani 1 1 d . . .
Cl7 Cl 0.90298(11) 0.04291(10) 0.64912(8) 0.0185(2) Uani 1 1 d . . .
Cl8 Cl 0.57667(12) -0.08228(11) 0.56356(9) 0.0214(2) Uani 1 1 d . . .
Cl9 Cl 0.50863(11) 0.14987(10) 0.43425(8) 0.0174(2) Uani 1 1 d . . .
Cl10 Cl 0.62590(12) 0.22828(11) 0.65983(9) 0.0213(2) Uani 1 1 d . . .
N4 N 0.7748(4) -0.0175(3) 0.4423(3) 0.0147(8) Uani 1 1 d . . .
N5 N 0.6847(4) -0.0914(4) 0.3674(3) 0.0173(8) Uani 1 1 d . . .
N6 N 0.9051(4) -0.1070(4) 0.3536(3) 0.0168(9) Uani 1 1 d . . .
H6 H 0.9789 -0.1297 0.3311 0.020 Uiso 1 1 calc R . .
C19 C 0.7664(5) -0.1438(5) 0.3155(4) 0.0190(10) Uani 1 1 d . . .
H19 H 0.7334 -0.1998 0.2590 0.023 Uiso 1 1 calc R . .
C20 C 0.9067(5) -0.0287(4) 0.4330(3) 0.0163(9) Uani 1 1 d . . .
H20 H 0.9891 0.0117 0.4751 0.020 Uiso 1 1 calc R . .
N8 N -0.0729(4) 0.6173(3) 0.7270(3) 0.0142(7) Uani 1 1 d . . .
C21 C -0.0436(5) 0.7598(4) 0.7679(4) 0.0183(10) Uani 1 1 d . . .
H21A H -0.1122 0.8128 0.7303 0.022 Uiso 1 1 calc R . .
H21B H -0.0605 0.7723 0.8305 0.022 Uiso 1 1 calc R . .
C22 C 0.1067(5) 0.8095(4) 0.7735(4) 0.0200(10) Uani 1 1 d . . .
H22A H 0.1161 0.8206 0.7114 0.024 Uiso 1 1 calc R . .
H22B H 0.1759 0.7449 0.7968 0.024 Uiso 1 1 calc R . .
C23 C 0.1405(5) 0.9397(5) 0.8374(4) 0.0232(11) Uani 1 1 d . . .
H23A H 0.0659 1.0016 0.8173 0.028 Uiso 1 1 calc R . .
H23B H 0.1391 0.9266 0.9007 0.028 Uiso 1 1 calc R . .
C24 C 0.2860(6) 0.9975(6) 0.8375(5) 0.0386(15) Uani 1 1 d . . .
H24A H 0.3034 1.0808 0.8783 0.058 Uiso 1 1 calc R . .
H24B H 0.2876 1.0110 0.7751 0.058 Uiso 1 1 calc R . .
H24C H 0.3604 0.9376 0.8593 0.058 Uiso 1 1 calc R . .
C25 C 0.0062(5) 0.5374(4) 0.7985(3) 0.0159(9) Uani 1 1 d . . .
H25A H -0.0269 0.5617 0.8555 0.019 Uiso 1 1 calc R . .
H25B H 0.1088 0.5622 0.8127 0.019 Uiso 1 1 calc R . .
C26 C -0.0098(5) 0.3902(4) 0.7728(4) 0.0210(10) Uani 1 1 d . . .
H26A H 0.0304 0.3622 0.7191 0.025 Uiso 1 1 calc R . .
H26B H -0.1119 0.3628 0.7563 0.025 Uiso 1 1 calc R . .
C27 C 0.0695(6) 0.3275(5) 0.8551(4) 0.0295(12) Uani 1 1 d . . .
H27A H 0.0286 0.3569 0.9083 0.035 Uiso 1 1 calc R . .
H27B H 0.0545 0.2320 0.8401 0.035 Uiso 1 1 calc R . .
C28 C 0.2294(6) 0.3608(6) 0.8819(5) 0.0405(16) Uani 1 1 d . . .
H28A H 0.2745 0.3190 0.9350 0.061 Uiso 1 1 calc R . .
H28B H 0.2450 0.4552 0.8977 0.061 Uiso 1 1 calc R . .
H28C H 0.2712 0.3295 0.8301 0.061 Uiso 1 1 calc R . .
C29 C -0.2334(5) 0.5866(5) 0.7037(4) 0.0205(10) Uani 1 1 d . . .
H29A H -0.2820 0.6499 0.6649 0.025 Uiso 1 1 calc R . .
H29B H -0.2522 0.4993 0.6666 0.025 Uiso 1 1 calc R . .
C30 C -0.2994(5) 0.5893(6) 0.7855(4) 0.0279(12) Uani 1 1 d . . .
H30A H -0.2774 0.6744 0.8252 0.034 Uiso 1 1 calc R . .
H30B H -0.2581 0.5210 0.8222 0.034 Uiso 1 1 calc R . .
C31 C -0.4624(6) 0.5662(6) 0.7528(5) 0.0331(13) Uani 1 1 d . . .
H31A H -0.4831 0.4866 0.7069 0.040 Uiso 1 1 calc R . .
H31B H -0.5005 0.5512 0.8058 0.040 Uiso 1 1 calc R . .
C32 C -0.5387(6) 0.6773(7) 0.7109(5) 0.0435(16) Uani 1 1 d . . .
H32A H -0.6413 0.6565 0.6921 0.065 Uiso 1 1 calc R . .
H32B H -0.5039 0.6913 0.6572 0.065 Uiso 1 1 calc R . .
H32C H -0.5206 0.7563 0.7562 0.065 Uiso 1 1 calc R . .
C33 C -0.0217(5) 0.5860(4) 0.6398(3) 0.0154(9) Uani 1 1 d . . .
H33A H -0.0411 0.4922 0.6167 0.018 Uiso 1 1 calc R . .
H33B H 0.0828 0.6014 0.6551 0.018 Uiso 1 1 calc R . .
C34 C -0.0876(5) 0.6621(5) 0.5628(4) 0.0207(10) Uani 1 1 d . . .
H34A H -0.0690 0.7563 0.5844 0.025 Uiso 1 1 calc R . .
H34B H -0.1920 0.6453 0.5448 0.025 Uiso 1 1 calc R . .
C35 C -0.0243(5) 0.6221(5) 0.4797(4) 0.0241(11) Uani 1 1 d . . .
H35A H -0.0323 0.5263 0.4641 0.029 Uiso 1 1 calc R . .
H35B H -0.0819 0.6589 0.4266 0.029 Uiso 1 1 calc R . .
C36 C 0.1310(6) 0.6655(7) 0.4940(4) 0.0363(14) Uani 1 1 d . . .
H36A H 0.1631 0.6369 0.4379 0.054 Uiso 1 1 calc R . .
H36B H 0.1896 0.6271 0.5451 0.054 Uiso 1 1 calc R . .
H36C H 0.1400 0.7605 0.5083 0.054 Uiso 1 1 calc R . .
O1 O 0.5941(4) 0.6568(4) 0.1279(3) 0.0324(9) Uani 1 1 d . . .
H1A H 0.6733 0.6877 0.1257 0.049 Uiso 1 1 calc R . .
C37 C 0.5054(6) 0.6281(6) 0.0366(4) 0.0293(13) Uani 1 1 d . . .
H37A H 0.4087 0.6011 0.0397 0.035 Uiso 1 1 calc R . .
H37B H 0.5448 0.5549 0.0021 0.035 Uiso 1 1 calc R . .
C38 C 0.4960(7) 0.7435(7) -0.0131(5) 0.0402(15) Uani 1 1 d . . .
H38A H 0.4612 0.8173 0.0224 0.060 Uiso 1 1 calc R . .
H38B H 0.4300 0.7227 -0.0736 0.060 Uiso 1 1 calc R . .
H38C H 0.5905 0.7660 -0.0207 0.060 Uiso 1 1 calc R . .
O2 O 1.2420(5) 0.0785(7) 0.5451(5) 0.087(3) Uani 1 1 d . . .
H2A H 1.3196 0.0409 0.5578 0.130 Uiso 1 1 calc R . .
C39 C 1.2411(7) 0.1863(7) 0.6152(5) 0.0466(19) Uani 1 1 d . . .
H39A H 1.3247 0.1823 0.6670 0.056 Uiso 1 1 calc R . .
H39B H 1.1545 0.1784 0.6386 0.056 Uiso 1 1 calc R . .
C40 C 1.2441(7) 0.3125(8) 0.5842(5) 0.0512(19) Uani 1 1 d . . .
H40A H 1.3264 0.3193 0.5576 0.077 Uiso 1 1 calc R . .
H40B H 1.2514 0.3816 0.6364 0.077 Uiso 1 1 calc R . .
H40C H 1.1564 0.3212 0.5376 0.077 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 0.0016 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Os1 Cl2 88.37(10) . . ?
N1 Os1 Cl1 88.23(10) . . ?
Cl2 Os1 Cl1 91.00(4) . . ?
N1 Os1 Cl4 88.96(10) . . ?
Cl2 Os1 Cl4 177.25(4) . . ?
Cl1 Os1 Cl4 89.56(4) . . ?
N1 Os1 Cl5 177.99(11) . . ?
Cl2 Os1 Cl5 89.63(4) . . ?
Cl1 Os1 Cl5 91.65(4) . . ?
Cl4 Os1 Cl5 93.05(4) . . ?
N1 Os1 Cl3 89.01(10) . . ?
Cl2 Os1 Cl3 89.76(4) . . ?
Cl1 Os1 Cl3 177.11(4) . . ?
Cl4 Os1 Cl3 89.55(4) . . ?
Cl5 Os1 Cl3 91.14(4) . . ?
C2 N1 N2 108.2(4) . . ?
C2 N1 Os1 129.5(3) . . ?
N2 N1 Os1 122.1(3) . . ?
C1 N2 N1 105.5(4) . . ?
C2 N3 C1 105.8(4) . . ?
C2 N3 H3 127.1 . . ?
C1 N3 H3 127.1 . . ?
N2 C1 N3 111.3(5) . . ?
N2 C1 H1 124.3 . . ?
N3 C1 H1 124.3 . . ?
N1 C2 N3 109.1(4) . . ?
N1 C2 H2 125.5 . . ?
N3 C2 H2 125.5 . . ?
C3 N7 C15 111.2(4) . . ?
C3 N7 C11 106.0(3) . . ?
C15 N7 C11 111.5(3) . . ?
C3 N7 C7 111.3(3) . . ?
C15 N7 C7 105.9(3) . . ?
C11 N7 C7 111.0(3) . . ?
N7 C3 C4 115.4(4) . . ?
N7 C3 H3A 108.4 . . ?
C4 C3 H3A 108.4 . . ?
N7 C3 H3B 108.4 . . ?
C4 C3 H3B 108.4 . . ?
H3A C3 H3B 107.5 . . ?
C5 C4 C3 110.7(4) . . ?
C5 C4 H4A 109.5 . . ?
C3 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
C6 C5 C4 111.6(5) . . ?
C6 C5 H5A 109.3 . . ?
C4 C5 H5A 109.3 . . ?
C6 C5 H5B 109.3 . . ?
C4 C5 H5B 109.3 . . ?
H5A C5 H5B 108.0 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 N7 115.0(3) . . ?
C8 C7 H7A 108.5 . . ?
N7 C7 H7A 108.5 . . ?
C8 C7 H7B 108.5 . . ?
N7 C7 H7B 108.5 . . ?
H7A C7 H7B 107.5 . . ?
C7 C8 C9 110.5(4) . . ?
C7 C8 H8A 109.5 . . ?
C9 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 108.1 . . ?
C10 C9 C8 111.7(4) . . ?
C10 C9 H9A 109.3 . . ?
C8 C9 H9A 109.3 . . ?
C10 C9 H9B 109.3 . . ?
C8 C9 H9B 109.3 . . ?
H9A C9 H9B 107.9 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 N7 116.9(4) . . ?
C12 C11 H11A 108.1 . . ?
N7 C11 H11A 108.1 . . ?
C12 C11 H11B 108.1 . . ?
N7 C11 H11B 108.1 . . ?
H11A C11 H11B 107.3 . . ?
C13 C12 C11 110.8(4) . . ?
C13 C12 H12A 109.5 . . ?
C11 C12 H12A 109.5 . . ?
C13 C12 H12B 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
C12 C13 C14 112.5(5) . . ?
C12 C13 H13A 109.1 . . ?
C14 C13 H13A 109.1 . . ?
C12 C13 H13B 109.1 . . ?
C14 C13 H13B 109.1 . . ?
H13A C13 H13B 107.8 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 N7 115.3(3) . . ?
C16 C15 H15A 108.5 . . ?
N7 C15 H15A 108.5 . . ?
C16 C15 H15B 108.5 . . ?
N7 C15 H15B 108.5 . . ?
H15A C15 H15B 107.5 . . ?
C15 C16 C17 111.0(4) . . ?
C15 C16 H16A 109.4 . . ?
C17 C16 H16A 109.4 . . ?
C15 C16 H16B 109.4 . . ?
C17 C16 H16B 109.4 . . ?
H16A C16 H16B 108.0 . . ?
C18 C17 C16 111.4(4) . . ?
C18 C17 H17A 109.3 . . ?
C16 C17 H17A 109.3 . . ?
C18 C17 H17B 109.3 . . ?
C16 C17 H17B 109.3 . . ?
H17A C17 H17B 108.0 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N4 Os2 Cl10 179.54(10) . . ?
N4 Os2 Cl7 88.02(10) . . ?
Cl10 Os2 Cl7 91.80(4) . . ?
N4 Os2 Cl8 88.57(10) . . ?
Cl10 Os2 Cl8 91.85(4) . . ?
Cl7 Os2 Cl8 90.72(4) . . ?
N4 Os2 Cl9 88.98(11) . . ?
Cl10 Os2 Cl9 91.19(4) . . ?
Cl7 Os2 Cl9 176.90(4) . . ?
Cl8 Os2 Cl9 90.00(4) . . ?
N4 Os2 Cl6 87.12(10) . . ?
Cl10 Os2 Cl6 92.45(4) . . ?
Cl7 Os2 Cl6 90.16(4) . . ?
Cl8 Os2 Cl6 175.58(4) . . ?
Cl9 Os2 Cl6 88.89(4) . . ?
C20 N4 N5 108.5(4) . . ?
C20 N4 Os2 127.8(3) . . ?
N5 N4 Os2 123.6(3) . . ?
C19 N5 N4 106.0(3) . . ?
C20 N6 C19 106.2(4) . . ?
C20 N6 H6 126.9 . . ?
C19 N6 H6 126.9 . . ?
N5 C19 N6 110.6(4) . . ?
N5 C19 H19 124.7 . . ?
N6 C19 H19 124.7 . . ?
N4 C20 N6 108.7(4) . . ?
N4 C20 H20 125.7 . . ?
N6 C20 H20 125.7 . . ?
C33 N8 C21 111.4(3) . . ?
C33 N8 C25 109.7(3) . . ?
C21 N8 C25 107.2(4) . . ?
C33 N8 C29 108.1(4) . . ?
C21 N8 C29 109.5(3) . . ?
C25 N8 C29 111.0(3) . . ?
C22 C21 N8 114.2(4) . . ?
C22 C21 H21A 108.7 . . ?
N8 C21 H21A 108.7 . . ?
C22 C21 H21B 108.7 . . ?
N8 C21 H21B 108.7 . . ?
H21A C21 H21B 107.6 . . ?
C21 C22 C23 110.8(4) . . ?
C21 C22 H22A 109.5 . . ?
C23 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C23 C22 H22B 109.5 . . ?
H22A C22 H22B 108.1 . . ?
C24 C23 C22 111.8(5) . . ?
C24 C23 H23A 109.3 . . ?
C22 C23 H23A 109.3 . . ?
C24 C23 H23B 109.3 . . ?
C22 C23 H23B 109.3 . . ?
H23A C23 H23B 107.9 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N8 C25 C26 116.4(4) . . ?
N8 C25 H25A 108.2 . . ?
C26 C25 H25A 108.2 . . ?
N8 C25 H25B 108.2 . . ?
C26 C25 H25B 108.2 . . ?
H25A C25 H25B 107.3 . . ?
C25 C26 C27 108.6(4) . . ?
C25 C26 H26A 110.0 . . ?
C27 C26 H26A 110.0 . . ?
C25 C26 H26B 110.0 . . ?
C27 C26 H26B 110.0 . . ?
H26A C26 H26B 108.3 . . ?
C28 C27 C26 112.9(5) . . ?
C28 C27 H27A 109.0 . . ?
C26 C27 H27A 109.0 . . ?
C28 C27 H27B 109.0 . . ?
C26 C27 H27B 109.0 . . ?
H27A C27 H27B 107.8 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 N8 115.6(4) . . ?
C30 C29 H29A 108.4 . . ?
N8 C29 H29A 108.4 . . ?
C30 C29 H29B 108.4 . . ?
N8 C29 H29B 108.4 . . ?
H29A C29 H29B 107.4 . . ?
C29 C30 C31 110.4(5) . . ?
C29 C30 H30A 109.6 . . ?
C31 C30 H30A 109.6 . . ?
C29 C30 H30B 109.6 . . ?
C31 C30 H30B 109.6 . . ?
H30A C30 H30B 108.1 . . ?
C32 C31 C30 113.8(5) . . ?
C32 C31 H31A 108.8 . . ?
C30 C31 H31A 108.8 . . ?
C32 C31 H31B 108.8 . . ?
C30 C31 H31B 108.8 . . ?
H31A C31 H31B 107.7 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N8 C33 C34 115.8(4) . . ?
N8 C33 H33A 108.3 . . ?
C34 C33 H33A 108.3 . . ?
N8 C33 H33B 108.3 . . ?
C34 C33 H33B 108.3 . . ?
H33A C33 H33B 107.4 . . ?
C33 C34 C35 110.1(4) . . ?
C33 C34 H34A 109.6 . . ?
C35 C34 H34A 109.6 . . ?
C33 C34 H34B 109.6 . . ?
C35 C34 H34B 109.6 . . ?
H34A C34 H34B 108.2 . . ?
C36 C35 C34 114.5(5) . . ?
C36 C35 H35A 108.6 . . ?
C34 C35 H35A 108.6 . . ?
C36 C35 H35B 108.6 . . ?
C34 C35 H35B 108.6 . . ?
H35A C35 H35B 107.6 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C37 O1 H1A 109.5 . . ?
O1 C37 C38 111.4(5) . . ?
O1 C37 H37A 109.4 . . ?
C38 C37 H37A 109.4 . . ?
O1 C37 H37B 109.4 . . ?
C38 C37 H37B 109.4 . . ?
H37A C37 H37B 108.0 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C39 O2 H2A 109.5 . . ?
O2 C39 C40 113.7(8) . . ?
O2 C39 H39A 108.8 . . ?
C40 C39 H39A 108.8 . . ?
O2 C39 H39B 108.8 . . ?
C40 C39 H39B 108.8 . . ?
H39A C39 H39B 107.7 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os1 N1 2.086(4) . ?
Os1 Cl2 2.3202(11) . ?
Os1 Cl1 2.3207(11) . ?
Os1 Cl4 2.3216(11) . ?
Os1 Cl5 2.3270(11) . ?
Os1 Cl3 2.3411(10) . ?
N1 C2 1.319(5) . ?
N1 N2 1.376(5) . ?
N2 C1 1.301(6) . ?
N3 C2 1.333(6) . ?
N3 C1 1.347(7) . ?
N3 H3 0.8800 . ?
C1 H1 0.9500 . ?
C2 H2 0.9500 . ?
N7 C3 1.524(6) . ?
N7 C15 1.526(5) . ?
N7 C11 1.529(6) . ?
N7 C7 1.530(5) . ?
C3 C4 1.531(7) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.517(7) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.510(8) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.519(6) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.522(6) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.519(7) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.515(7) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.513(7) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.524(8) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.511(6) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.524(6) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.516(7) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
Os2 N4 2.081(4) . ?
Os2 Cl10 2.3136(12) . ?
Os2 Cl7 2.3137(11) . ?
Os2 Cl8 2.3288(11) . ?
Os2 Cl9 2.3289(11) . ?
Os2 Cl6 2.3395(10) . ?
N4 C20 1.319(6) . ?
N4 N5 1.386(6) . ?
N5 C19 1.307(6) . ?
N6 C20 1.349(6) . ?
N6 C19 1.360(7) . ?
N6 H6 0.8800 . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
N8 C33 1.511(6) . ?
N8 C21 1.522(6) . ?
N8 C25 1.522(6) . ?
N8 C29 1.531(6) . ?
C21 C22 1.521(6) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.535(7) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.530(8) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.525(6) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.532(7) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.529(8) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.519(7) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.544(7) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.507(9) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.519(6) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.531(7) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.524(7) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
O1 C37 1.434(7) . ?
O1 H1A 0.8400 . ?
C37 C38 1.498(8) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
O2 C39 1.433(8) . ?
O2 H2A 0.8400 . ?
C39 C40 1.459(11) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
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
Cl2 Os1 N1 C2 132.4(4) . . . . ?
Cl1 Os1 N1 C2 41.4(4) . . . . ?
Cl4 Os1 N1 C2 -48.2(4) . . . . ?
Cl3 Os1 N1 C2 -137.8(4) . . . . ?
Cl2 Os1 N1 N2 -41.7(3) . . . . ?
Cl1 Os1 N1 N2 -132.7(3) . . . . ?
Cl4 Os1 N1 N2 137.7(3) . . . . ?
Cl3 Os1 N1 N2 48.1(3) . . . . ?
C2 N1 N2 C1 -0.1(5) . . . . ?
Os1 N1 N2 C1 175.1(3) . . . . ?
N1 N2 C1 N3 0.6(6) . . . . ?
C2 N3 C1 N2 -0.8(6) . . . . ?
N2 N1 C2 N3 -0.4(5) . . . . ?
Os1 N1 C2 N3 -175.2(3) . . . . ?
C1 N3 C2 N1 0.8(5) . . . . ?
C15 N7 C3 C4 -62.9(5) . . . . ?
C11 N7 C3 C4 175.8(4) . . . . ?
C7 N7 C3 C4 55.0(5) . . . . ?
N7 C3 C4 C5 174.3(4) . . . . ?
C3 C4 C5 C6 174.5(4) . . . . ?
C3 N7 C7 C8 58.7(5) . . . . ?
C15 N7 C7 C8 179.7(4) . . . . ?
C11 N7 C7 C8 -59.2(5) . . . . ?
N7 C7 C8 C9 -176.9(4) . . . . ?
C7 C8 C9 C10 176.4(4) . . . . ?
C3 N7 C11 C12 -177.7(4) . . . . ?
C15 N7 C11 C12 61.1(5) . . . . ?
C7 N7 C11 C12 -56.6(5) . . . . ?
N7 C11 C12 C13 -177.6(4) . . . . ?
C11 C12 C13 C14 -180.0(4) . . . . ?
C3 N7 C15 C16 -53.5(5) . . . . ?
C11 N7 C15 C16 64.6(5) . . . . ?
C7 N7 C15 C16 -174.6(4) . . . . ?
N7 C15 C16 C17 -171.9(4) . . . . ?
C15 C16 C17 C18 179.4(5) . . . . ?
Cl7 Os2 N4 C20 -40.1(4) . . . . ?
Cl8 Os2 N4 C20 -130.9(4) . . . . ?
Cl9 Os2 N4 C20 139.1(4) . . . . ?
Cl6 Os2 N4 C20 50.2(4) . . . . ?
Cl7 Os2 N4 N5 144.0(3) . . . . ?
Cl8 Os2 N4 N5 53.3(3) . . . . ?
Cl9 Os2 N4 N5 -36.8(3) . . . . ?
Cl6 Os2 N4 N5 -125.7(3) . . . . ?
C20 N4 N5 C19 -0.3(5) . . . . ?
Os2 N4 N5 C19 176.2(3) . . . . ?
N4 N5 C19 N6 0.0(5) . . . . ?
C20 N6 C19 N5 0.3(5) . . . . ?
N5 N4 C20 N6 0.5(5) . . . . ?
Os2 N4 C20 N6 -175.9(3) . . . . ?
C19 N6 C20 N4 -0.5(5) . . . . ?
C33 N8 C21 C22 -47.2(5) . . . . ?
C25 N8 C21 C22 72.8(5) . . . . ?
C29 N8 C21 C22 -166.7(4) . . . . ?
N8 C21 C22 C23 -165.0(4) . . . . ?
C21 C22 C23 C24 -175.0(4) . . . . ?
C33 N8 C25 C26 -59.8(5) . . . . ?
C21 N8 C25 C26 179.1(4) . . . . ?
C29 N8 C25 C26 59.6(5) . . . . ?
N8 C25 C26 C27 -176.6(4) . . . . ?
C25 C26 C27 C28 -62.1(6) . . . . ?
C33 N8 C29 C30 169.6(4) . . . . ?
C21 N8 C29 C30 -68.9(5) . . . . ?
C25 N8 C29 C30 49.2(5) . . . . ?
N8 C29 C30 C31 176.0(4) . . . . ?
C29 C30 C31 C32 -69.5(7) . . . . ?
C21 N8 C33 C34 -59.4(5) . . . . ?
C25 N8 C33 C34 -177.9(4) . . . . ?
C29 N8 C33 C34 61.0(5) . . . . ?
N8 C33 C34 C35 179.0(4) . . . . ?
C33 C34 C35 C36 -69.8(6) . . . . ?
