#------------------------------------------------------------------------------
#$Date: 2020-07-06 05:07:08 +0200 (lun 06 de jul de 2020) $
#$Revision: 253897 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/46/7704640.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_7704640
loop_
_publ_author_name
'Gianino, Jacqueline'
'Erickson, Alexander N.'
'Markovitz, Sean J.'
'Brown, Seth N.'
_publ_section_title
;
 High-valent osmium iminoxolene complexes.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8504
_journal_page_last               8515
_journal_paper_doi               10.1039/d0dt01735c
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C44 H52 N2 O7 Os'
_chemical_formula_sum            'C44 H52 N2 O7 Os'
_chemical_formula_weight         911.07
_chemical_name_common            (Egan)OsO
_chemical_name_systematic
(Oxo)(1,2-ethanedi-(2-(3,5-di-tert-butyl-2-oxyphenyl)amido)-benzoate)osmium(VI)
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2020-05-11 deposited with the CCDC.	2020-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                105.229(2)
_cell_angle_beta                 104.4965(19)
_cell_angle_gamma                108.180(2)
_cell_formula_units_Z            2
_cell_length_a                   13.0153(6)
_cell_length_b                   13.1218(7)
_cell_length_c                   14.0466(6)
_cell_measurement_reflns_used    9775
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30.64
_cell_measurement_theta_min      2.50
_cell_volume                     2049.60(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            66041
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.659
_diffrn_reflns_theta_min         1.612
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.162
_exptl_absorpt_correction_T_max  0.7802
_exptl_absorpt_correction_T_min  0.6140
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             924
_exptl_crystal_recrystallization_method
'Crystals were grown by vapor diffusion of methanol intoa benzene solution of the complex.'
_exptl_crystal_size_max          0.214
_exptl_crystal_size_mid          0.129
_exptl_crystal_size_min          0.120
_exptl_transmission_factor_max   0.7802
_exptl_transmission_factor_min   0.6140
_refine_diff_density_max         0.533
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     88
_refine_ls_number_reflns         12637
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0156
_refine_ls_R_factor_gt           0.0140
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0160P)²+0.7482P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0332
_refine_ls_wR_factor_ref         0.0336
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11999
_reflns_number_total             12637
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt01735c2.cif
_cod_data_source_block           eganoso
_cod_depositor_comments
'Adding full bibliography for 7704635--7704640.cif.'
_cod_original_cell_volume        2049.60(17)
_cod_database_code               7704640
_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. 
;
_shelx_estimated_absorpt_t_min   0.551
_shelx_estimated_absorpt_t_max   0.703
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-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_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 0.97083(2) 0.91603(2) 0.71251(2) 0.01122(2) Uani 1 1 d . . . . .
O O 1.00751(8) 1.06044(8) 0.75597(8) 0.01992(19) Uani 1 1 d . . . . .
O1 O 1.11099(7) 0.88958(8) 0.73876(7) 0.01379(16) Uani 1 1 d . . . . .
N1 N 0.96508(9) 0.86012(9) 0.82583(8) 0.01312(19) Uani 1 1 d . . . . .
C1 C 0.87670(12) 0.53281(12) 0.64354(11) 0.0189(2) Uani 1 1 d . . . . .
H1B H 0.9546(15) 0.5472(15) 0.6793(13) 0.021(4) Uiso 1 1 d . . . . .
H1A H 0.8269(15) 0.4630(16) 0.6416(13) 0.024(4) Uiso 1 1 d . . . . .
O2 O 0.80360(7) 0.83717(8) 0.65392(7) 0.01348(16) Uani 1 1 d . . . . .
N2 N 0.94865(9) 0.85627(9) 0.56449(8) 0.01241(18) Uani 1 1 d . . . . .
C2 C 0.85566(12) 0.52989(12) 0.53326(11) 0.0196(3) Uani 1 1 d . . . . .
H2B H 0.7805(15) 0.5257(14) 0.5021(13) 0.020(4) Uiso 1 1 d . . . . .
H2A H 0.8627(16) 0.4648(17) 0.4904(15) 0.030(5) Uiso 1 1 d . . . . .
O10 O 0.80367(13) 0.52519(10) 0.80151(10) 0.0400(3) Uani 1 1 d . . . . .
O11 O 0.85303(8) 0.62551(8) 0.70182(7) 0.01702(17) Uani 1 1 d . . . . .
C11 C 1.14152(10) 0.85721(10) 0.82294(9) 0.0133(2) Uani 1 1 d . . . . .
C12 C 1.06022(10) 0.83637(11) 0.87072(9) 0.0135(2) Uani 1 1 d . . . . .
C13 C 1.07579(11) 0.79507(11) 0.95252(10) 0.0161(2) Uani 1 1 d . . . . .
H13 H 1.0183(15) 0.7820(15) 0.9850(14) 0.024(4) Uiso 1 1 d . . . . .
C14 C 1.17535(11) 0.77608(11) 0.98702(10) 0.0172(2) Uani 1 1 d . . . . .
C15 C 1.25812(11) 0.80228(12) 0.93976(10) 0.0171(2) Uani 1 1 d . . . . .
H15 H 1.3272(14) 0.7910(14) 0.9651(12) 0.015(4) Uiso 1 1 d . . . . .
C16 C 1.24418(10) 0.84207(11) 0.85662(9) 0.0144(2) Uani 1 1 d . . . . .
C17 C 1.33182(11) 0.86308(12) 0.80175(10) 0.0173(2) Uani 1 1 d . . . . .
C18 C 1.19465(12) 0.72194(14) 1.07037(11) 0.0238(3) Uani 1 1 d . . . . .
O20 O 0.91334(9) 0.55107(9) 0.36706(8) 0.0252(2) Uani 1 1 d . . . . .
O21 O 0.93952(8) 0.63485(8) 0.53804(7) 0.01728(18) Uani 1 1 d . . . . .
C21 C 0.75430(10) 0.78906(10) 0.54589(9) 0.0130(2) Uani 1 1 d . . . . .
C22 C 0.83286(10) 0.79595(10) 0.49423(9) 0.0128(2) Uani 1 1 d . . . . .
C23 C 0.79540(11) 0.74806(11) 0.38477(10) 0.0151(2) Uani 1 1 d . . . . .
H23 H 0.8521(14) 0.7566(14) 0.3518(13) 0.017(4) Uiso 1 1 d . . . . .
C24 C 0.67732(11) 0.68946(11) 0.32621(10) 0.0169(2) Uani 1 1 d . . . . .
C25 C 0.60002(11) 0.68593(12) 0.38021(10) 0.0177(2) Uani 1 1 d . . . . .
H25 H 0.5173(14) 0.6471(14) 0.3395(13) 0.017(4) Uiso 1 1 d . . . . .
C26 C 0.63451(10) 0.73633(11) 0.48981(10) 0.0151(2) Uani 1 1 d . . . . .
C27 C 0.54803(11) 0.73902(12) 0.54565(10) 0.0177(2) Uani 1 1 d . . . . .
C28 C 0.63268(12) 0.62299(13) 0.20701(10) 0.0223(3) Uani 1 1 d . . . . .
C30 C 0.82131(12) 0.61183(12) 0.78287(10) 0.0192(2) Uani 1 1 d . . . . .
C31 C 0.80422(11) 0.71302(11) 0.84282(10) 0.0162(2) Uani 1 1 d . . . . .
C32 C 0.86664(10) 0.82683(11) 0.85557(9) 0.0145(2) Uani 1 1 d . . . . .
C33 C 0.83640(11) 0.91349(12) 0.90378(10) 0.0193(2) Uani 1 1 d . . . . .
H33 H 0.8736(16) 0.9875(17) 0.9107(14) 0.029(5) Uiso 1 1 d . . . . .
C34 C 0.74686(12) 0.88891(14) 0.94230(11) 0.0236(3) Uani 1 1 d . . . . .
H34 H 0.7285(15) 0.9475(16) 0.9752(14) 0.026(4) Uiso 1 1 d . . . . .
C35 C 0.68913(12) 0.77732(14) 0.93465(11) 0.0245(3) Uani 1 1 d . . . . .
H35 H 0.6289(16) 0.7586(16) 0.9596(15) 0.032(5) Uiso 1 1 d . . . . .
C36 C 0.71777(12) 0.69033(13) 0.88556(11) 0.0213(3) Uani 1 1 d . . . . .
H36 H 0.6794(15) 0.6151(15) 0.8776(13) 0.020(4) Uiso 1 1 d . . . . .
C40 C 0.95559(11) 0.63498(12) 0.44742(10) 0.0175(2) Uani 1 1 d . . . . .
C41 C 1.03804(11) 0.75091(11) 0.46239(10) 0.0166(2) Uani 1 1 d . . . . .
C42 C 1.03882(10) 0.85368(11) 0.52524(10) 0.0142(2) Uani 1 1 d . . . . .
C43 C 1.12768(11) 0.95796(12) 0.54725(11) 0.0184(2) Uani 1 1 d . . . . .
H43 H 1.1319(15) 1.0264(16) 0.5901(14) 0.026(4) Uiso 1 1 d . . . . .
C44 C 1.21337(13) 0.96128(14) 0.50446(13) 0.0252(3) Uani 1 1 d . . . . .
H44 H 1.2725(16) 1.0295(16) 0.5201(14) 0.029(5) Uiso 1 1 d . . . . .
C45 C 1.20814(14) 0.86103(15) 0.43632(13) 0.0279(3) Uani 1 1 d . . . . .
H45 H 1.2649(17) 0.8668(17) 0.4069(15) 0.034(5) Uiso 1 1 d . . . . .
C46 C 1.12039(13) 0.75623(14) 0.41484(12) 0.0234(3) Uani 1 1 d . . . . .
H46 H 1.1171(15) 0.6878(16) 0.3684(14) 0.024(4) Uiso 1 1 d . . . . .
C171 C 1.27406(13) 0.77443(15) 0.68805(11) 0.0249(3) Uani 1 1 d . . . . .
H17C H 1.2050(17) 0.7804(16) 0.6503(15) 0.030(5) Uiso 1 1 d . . . . .
H17B H 1.2545(17) 0.6985(18) 0.6890(15) 0.036(5) Uiso 1 1 d . . . . .
H17A H 1.3272(18) 0.7843(18) 0.6491(16) 0.040(5) Uiso 1 1 d . . . . .
C172 C 1.44056(12) 0.84798(15) 0.85609(12) 0.0243(3) Uani 1 1 d . . . . .
H17F H 1.4793(15) 0.9029(16) 0.9284(14) 0.026(4) Uiso 1 1 d . . . . .
H17E H 1.4227(15) 0.7687(16) 0.8553(14) 0.026(5) Uiso 1 1 d . . . . .
H17D H 1.4947(16) 0.8618(16) 0.8196(14) 0.029(5) Uiso 1 1 d . . . . .
C173 C 1.36968(12) 0.98591(14) 0.80123(12) 0.0240(3) Uani 1 1 d . . . . .
H17I H 1.3056(16) 1.0047(16) 0.7657(14) 0.028(5) Uiso 1 1 d . . . . .
H17H H 1.4100(17) 1.0444(17) 0.8728(16) 0.033(5) Uiso 1 1 d . . . . .
H17G H 1.4243(18) 0.9986(17) 0.7649(16) 0.038(5) Uiso 1 1 d . . . . .
C181 C 1.2060(2) 0.60913(17) 1.02004(17) 0.0400(4) Uani 1 1 d . . . . .
H18C H 1.2141(18) 0.5729(18) 1.0721(16) 0.041(6) Uiso 1 1 d . . . . .
H18B H 1.1354(19) 0.5561(19) 0.9584(18) 0.045(6) Uiso 1 1 d . . . . .
H18A H 1.2720(18) 0.6224(18) 0.9925(16) 0.040(5) Uiso 1 1 d . . . . .
C182 C 1.09422(16) 0.6940(2) 1.10990(16) 0.0386(4) Uani 1 1 d . . . . .
H18F H 1.0225(18) 0.6423(17) 1.0515(16) 0.037(5) Uiso 1 1 d . . . . .
H18E H 1.0878(18) 0.7642(19) 1.1461(16) 0.041(6) Uiso 1 1 d . . . . .
H18D H 1.1068(18) 0.6576(18) 1.1596(16) 0.041(6) Uiso 1 1 d . . . . .
C183 C 1.30623(16) 0.80338(19) 1.16481(14) 0.0379(4) Uani 1 1 d . . . . .
H18I H 1.3176(19) 0.768(2) 1.2150(18) 0.051(6) Uiso 1 1 d . . . . .
H18H H 1.3748(19) 0.8234(19) 1.1439(17) 0.046(6) Uiso 1 1 d . . . . .
H18G H 1.2992(17) 0.8728(19) 1.1969(16) 0.037(6) Uiso 1 1 d . . . . .
C271 C 0.42294(12) 0.68014(15) 0.46714(12) 0.0260(3) Uani 1 1 d . . . . .
H27C H 0.4103(16) 0.7156(16) 0.4184(15) 0.027(5) Uiso 1 1 d . . . . .
H27B H 0.3712(17) 0.6858(16) 0.5048(15) 0.032(5) Uiso 1 1 d . . . . .
H27A H 0.4018(16) 0.6000(18) 0.4309(15) 0.033(5) Uiso 1 1 d . . . . .
C272 C 0.57279(13) 0.86516(14) 0.60498(13) 0.0253(3) Uani 1 1 d . . . . .
H27F H 0.6503(16) 0.9075(15) 0.6569(14) 0.026(4) Uiso 1 1 d . . . . .
H27E H 0.5206(16) 0.8698(16) 0.6399(15) 0.029(5) Uiso 1 1 d . . . . .
H27D H 0.5626(16) 0.9020(17) 0.5575(15) 0.031(5) Uiso 1 1 d . . . . .
C273 C 0.55903(13) 0.67703(15) 0.62369(12) 0.0255(3) Uani 1 1 d . . . . .
H27I H 0.6347(17) 0.7136(16) 0.6779(15) 0.031(5) Uiso 1 1 d . . . . .
H27H H 0.5478(17) 0.5995(18) 0.5904(15) 0.034(5) Uiso 1 1 d . . . . .
H27G H 0.5037(17) 0.6796(17) 0.6591(15) 0.035(5) Uiso 1 1 d . . . . .
C281 C 0.52660(18) 0.6404(2) 0.15008(13) 0.0397(4) Uani 1 1 d . . . . .
H28C H 0.5464(17) 0.7197(19) 0.1638(15) 0.034(5) Uiso 1 1 d . . . . .
H28B H 0.4999(18) 0.6015(19) 0.0765(18) 0.045(6) Uiso 1 1 d . . . . .
H28A H 0.462(2) 0.6167(19) 0.1742(17) 0.049(6) Uiso 1 1 d . . . . .
C282 C 0.72487(16) 0.65865(18) 0.15926(12) 0.0370(4) Uani 1 1 d . . . . .
H28F H 0.7508(17) 0.7404(18) 0.1723(15) 0.035(5) Uiso 1 1 d . . . . .
H28E H 0.792(2) 0.6449(19) 0.1876(17) 0.047(6) Uiso 1 1 d . . . . .
H28D H 0.6893(18) 0.6140(18) 0.0796(17) 0.043(6) Uiso 1 1 d . . . . .
C283 C 0.59902(16) 0.49477(15) 0.18960(13) 0.0321(3) Uani 1 1 d . . . . .
H28I H 0.6684(18) 0.4799(18) 0.2229(16) 0.039(5) Uiso 1 1 d . . . . .
H28H H 0.5687(17) 0.4466(17) 0.1151(16) 0.038(5) Uiso 1 1 d . . . . .
H28G H 0.5381(17) 0.4657(17) 0.2195(15) 0.035(5) Uiso 1 1 d . . . . .
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'
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
O Os O1 108.56(4) . . ?
O Os N1 110.68(5) . . ?
O1 Os N1 80.54(4) . . ?
O Os N2 110.63(5) . . ?
O1 Os N2 86.04(4) . . ?
N1 Os N2 138.69(4) . . ?
O Os O2 108.78(4) . . ?
O1 Os O2 142.66(4) . . ?
N1 Os O2 86.68(4) . . ?
N2 Os O2 80.77(4) . . ?
C11 O1 Os 116.26(7) . . ?
C12 N1 C32 118.78(10) . . ?
C12 N1 Os 115.92(8) . . ?
C32 N1 Os 124.68(8) . . ?
O11 C1 C2 108.71(11) . . ?
O11 C1 H1B 107.4(10) . . ?
C2 C1 H1B 111.9(10) . . ?
O11 C1 H1A 109.2(11) . . ?
C2 C1 H1A 109.2(11) . . ?
H1B C1 H1A 110.3(15) . . ?
C21 O2 Os 115.91(7) . . ?
C22 N2 C42 118.91(10) . . ?
C22 N2 Os 115.73(8) . . ?
C42 N2 Os 124.58(8) . . ?
O21 C2 C1 108.02(11) . . ?
O21 C2 H2B 108.8(10) . . ?
C1 C2 H2B 110.6(10) . . ?
O21 C2 H2A 110.0(11) . . ?
C1 C2 H2A 111.0(11) . . ?
H2B C2 H2A 108.3(15) . . ?
C30 O11 C1 115.34(10) . . ?
O1 C11 C12 114.64(10) . . ?
O1 C11 C16 123.32(11) . . ?
C12 C11 C16 122.00(11) . . ?
C11 C12 C13 121.00(11) . . ?
C11 C12 N1 112.32(10) . . ?
C13 C12 N1 126.67(11) . . ?
C14 C13 C12 119.01(12) . . ?
C14 C13 H13 121.5(10) . . ?
C12 C13 H13 119.4(10) . . ?
C13 C14 C15 118.57(12) . . ?
C13 C14 C18 122.27(12) . . ?
C15 C14 C18 119.09(12) . . ?
C16 C15 C14 123.71(12) . . ?
C16 C15 H15 118.1(10) . . ?
C14 C15 H15 118.2(9) . . ?
C15 C16 C11 115.63(11) . . ?
C15 C16 C17 122.93(11) . . ?
C11 C16 C17 121.39(11) . . ?
C16 C17 C172 112.16(11) . . ?
C16 C17 C171 108.01(11) . . ?
C172 C17 C171 108.05(12) . . ?
C16 C17 C173 110.52(11) . . ?
C172 C17 C173 107.98(11) . . ?
C171 C17 C173 110.09(12) . . ?
C182 C18 C183 108.73(14) . . ?
C182 C18 C14 112.33(12) . . ?
C183 C18 C14 110.20(13) . . ?
C182 C18 C181 108.29(15) . . ?
C183 C18 C181 108.97(15) . . ?
C14 C18 C181 108.24(12) . . ?
C40 O21 C2 116.46(10) . . ?
O2 C21 C22 114.75(10) . . ?
O2 C21 C26 123.72(11) . . ?
C22 C21 C26 121.52(11) . . ?
C23 C22 C21 121.16(11) . . ?
C23 C22 N2 126.22(11) . . ?
C21 C22 N2 112.62(10) . . ?
C22 C23 C24 119.26(11) . . ?
C22 C23 H23 118.8(10) . . ?
C24 C23 H23 121.9(10) . . ?
C23 C24 C25 118.31(11) . . ?
C23 C24 C28 121.04(12) . . ?
C25 C24 C28 120.50(12) . . ?
C26 C25 C24 123.92(12) . . ?
C26 C25 H25 117.4(10) . . ?
C24 C25 H25 118.7(9) . . ?
C25 C26 C21 115.70(11) . . ?
C25 C26 C27 122.61(11) . . ?
C21 C26 C27 121.64(11) . . ?
C271 C27 C26 111.76(11) . . ?
C271 C27 C272 108.11(12) . . ?
C26 C27 C272 108.68(11) . . ?
C271 C27 C273 107.90(12) . . ?
C26 C27 C273 110.53(11) . . ?
C272 C27 C273 109.82(12) . . ?
C282 C28 C24 112.38(12) . . ?
C282 C28 C281 108.77(14) . . ?
C24 C28 C281 110.82(13) . . ?
C282 C28 C283 107.97(14) . . ?
C24 C28 C283 107.19(11) . . ?
C281 C28 C283 109.65(14) . . ?
O10 C30 O11 123.32(13) . . ?
O10 C30 C31 124.06(13) . . ?
O11 C30 C31 112.53(11) . . ?
C36 C31 C32 119.07(13) . . ?
C36 C31 C30 116.78(12) . . ?
C32 C31 C30 124.13(11) . . ?
C33 C32 C31 119.62(12) . . ?
C33 C32 N1 117.31(12) . . ?
C31 C32 N1 123.00(11) . . ?
C32 C33 C34 120.63(14) . . ?
C32 C33 H33 121.4(12) . . ?
C34 C33 H33 118.0(12) . . ?
C35 C34 C33 119.71(14) . . ?
C35 C34 H34 120.5(11) . . ?
C33 C34 H34 119.7(12) . . ?
C36 C35 C34 119.96(13) . . ?
C36 C35 H35 118.6(12) . . ?
C34 C35 H35 121.4(12) . . ?
C35 C36 C31 120.86(14) . . ?
C35 C36 H36 121.8(11) . . ?
C31 C36 H36 117.3(11) . . ?
O20 C40 O21 124.26(13) . . ?
O20 C40 C41 125.11(12) . . ?
O21 C40 C41 110.53(11) . . ?
C46 C41 C42 119.21(12) . . ?
C46 C41 C40 117.96(12) . . ?
C42 C41 C40 122.78(11) . . ?
C43 C42 C41 119.55(12) . . ?
C43 C42 N2 117.90(12) . . ?
C41 C42 N2 122.49(11) . . ?
C42 C43 C44 120.38(14) . . ?
C42 C43 H43 121.5(11) . . ?
C44 C43 H43 118.1(11) . . ?
C45 C44 C43 120.14(14) . . ?
C45 C44 H44 119.5(12) . . ?
C43 C44 H44 120.4(12) . . ?
C44 C45 C46 119.81(13) . . ?
C44 C45 H45 117.9(12) . . ?
C46 C45 H45 122.3(12) . . ?
C45 C46 C41 120.57(14) . . ?
C45 C46 H46 119.7(11) . . ?
C41 C46 H46 119.7(11) . . ?
C17 C171 H17C 111.4(11) . . ?
C17 C171 H17B 109.6(12) . . ?
H17C C171 H17B 109.1(16) . . ?
C17 C171 H17A 111.2(12) . . ?
H17C C171 H17A 108.8(16) . . ?
H17B C171 H17A 106.6(17) . . ?
C17 C172 H17F 110.2(11) . . ?
C17 C172 H17E 112.1(10) . . ?
H17F C172 H17E 109.6(14) . . ?
C17 C172 H17D 110.4(11) . . ?
H17F C172 H17D 107.8(15) . . ?
H17E C172 H17D 106.5(15) . . ?
C17 C173 H17I 114.9(11) . . ?
C17 C173 H17H 111.9(11) . . ?
H17I C173 H17H 106.7(15) . . ?
C17 C173 H17G 110.4(12) . . ?
H17I C173 H17G 106.3(15) . . ?
H17H C173 H17G 106.1(16) . . ?
C18 C181 H18C 108.0(13) . . ?
C18 C181 H18B 110.2(13) . . ?
H18C C181 H18B 108.0(18) . . ?
C18 C181 H18A 111.9(12) . . ?
H18C C181 H18A 112.8(17) . . ?
H18B C181 H18A 105.9(17) . . ?
C18 C182 H18F 110.3(12) . . ?
C18 C182 H18E 110.3(13) . . ?
H18F C182 H18E 110.2(17) . . ?
C18 C182 H18D 110.8(13) . . ?
H18F C182 H18D 108.2(17) . . ?
H18E C182 H18D 106.9(17) . . ?
C18 C183 H18I 109.0(14) . . ?
C18 C183 H18H 112.3(13) . . ?
H18I C183 H18H 109.4(19) . . ?
C18 C183 H18G 109.3(13) . . ?
H18I C183 H18G 108.8(18) . . ?
H18H C183 H18G 108.0(18) . . ?
C27 C271 H27C 111.9(11) . . ?
C27 C271 H27B 109.4(11) . . ?
H27C C271 H27B 106.8(16) . . ?
C27 C271 H27A 111.3(11) . . ?
H27C C271 H27A 110.0(16) . . ?
H27B C271 H27A 107.1(16) . . ?
C27 C272 H27F 112.6(11) . . ?
C27 C272 H27E 110.8(12) . . ?
H27F C272 H27E 107.9(15) . . ?
C27 C272 H27D 110.1(12) . . ?
H27F C272 H27D 108.4(16) . . ?
H27E C272 H27D 106.7(16) . . ?
C27 C273 H27I 111.7(11) . . ?
C27 C273 H27H 112.3(12) . . ?
H27I C273 H27H 105.9(16) . . ?
C27 C273 H27G 109.8(11) . . ?
H27I C273 H27G 106.9(16) . . ?
H27H C273 H27G 110.2(16) . . ?
C28 C281 H28C 109.6(12) . . ?
C28 C281 H28B 111.3(13) . . ?
H28C C281 H28B 108.1(17) . . ?
C28 C281 H28A 114.1(13) . . ?
H28C C281 H28A 104.7(18) . . ?
H28B C281 H28A 108.7(18) . . ?
C28 C282 H28F 109.8(12) . . ?
C28 C282 H28E 113.5(13) . . ?
H28F C282 H28E 107.4(18) . . ?
C28 C282 H28D 108.8(12) . . ?
H28F C282 H28D 108.5(16) . . ?
H28E C282 H28D 108.7(17) . . ?
C28 C283 H28I 111.5(12) . . ?
C28 C283 H28H 112.0(12) . . ?
H28I C283 H28H 105.5(16) . . ?
C28 C283 H28G 111.9(11) . . ?
H28I C283 H28G 108.4(16) . . ?
H28H C283 H28G 107.3(16) . . ?
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 O 1.6951(9) . ?
Os O1 1.9260(9) . ?
Os N1 1.9277(10) . ?
Os N2 1.9295(10) . ?
Os O2 1.9328(9) . ?
O1 C11 1.3676(14) . ?
N1 C12 1.4076(15) . ?
N1 C32 1.4217(15) . ?
C1 O11 1.4428(16) . ?
C1 C2 1.4918(19) . ?
C1 H1B 0.945(17) . ?
C1 H1A 0.932(18) . ?
O2 C21 1.3673(14) . ?
N2 C22 1.4044(15) . ?
N2 C42 1.4218(15) . ?
C2 O21 1.4385(16) . ?
C2 H2B 0.944(17) . ?
C2 H2A 0.953(19) . ?
O10 C30 1.1988(17) . ?
O11 C30 1.3399(15) . ?
C11 C12 1.3843(17) . ?
C11 C16 1.3954(17) . ?
C12 C13 1.3908(17) . ?
C13 C14 1.3880(18) . ?
C13 H13 0.963(18) . ?
C14 C15 1.4022(18) . ?
C14 C18 1.5296(18) . ?
C15 C16 1.3937(17) . ?
C15 H15 0.953(16) . ?
C16 C17 1.5254(17) . ?
C17 C172 1.5292(18) . ?
C17 C171 1.5317(19) . ?
C17 C173 1.534(2) . ?
C18 C182 1.524(2) . ?
C18 C183 1.527(2) . ?
C18 C181 1.533(3) . ?
O20 C40 1.2030(16) . ?
O21 C40 1.3411(15) . ?
C21 C22 1.3885(16) . ?
C21 C26 1.3985(16) . ?
C22 C23 1.3866(17) . ?
C23 C24 1.3882(18) . ?
C23 H23 0.958(17) . ?
C24 C25 1.4004(18) . ?
C24 C28 1.5269(18) . ?
C25 C26 1.3939(17) . ?
C25 H25 0.971(16) . ?
C26 C27 1.5282(17) . ?
C27 C271 1.5272(18) . ?
C27 C272 1.532(2) . ?
C27 C273 1.532(2) . ?
C28 C282 1.525(2) . ?
C28 C281 1.529(2) . ?
C28 C283 1.534(2) . ?
C30 C31 1.4875(19) . ?
C31 C36 1.3921(18) . ?
C31 C32 1.3971(18) . ?
C32 C33 1.3838(19) . ?
C33 C34 1.3885(19) . ?
C33 H33 0.906(19) . ?
C34 C35 1.382(2) . ?
C34 H34 0.920(19) . ?
C35 C36 1.378(2) . ?
C35 H35 0.927(19) . ?
C36 H36 0.919(17) . ?
C40 C41 1.4867(18) . ?
C41 C46 1.3914(18) . ?
C41 C42 1.3998(18) . ?
C42 C43 1.3845(18) . ?
C43 C44 1.3879(19) . ?
C43 H43 0.917(19) . ?
C44 C45 1.379(2) . ?
C44 H44 0.907(19) . ?
C45 C46 1.384(2) . ?
C45 H45 0.93(2) . ?
C46 H46 0.943(18) . ?
C171 H17C 0.961(19) . ?
C171 H17B 0.95(2) . ?
C171 H17A 0.98(2) . ?
C172 H17F 0.968(18) . ?
C172 H17E 0.989(19) . ?
C172 H17D 0.970(19) . ?
C173 H17I 0.995(19) . ?
C173 H17H 0.98(2) . ?
C173 H17G 0.97(2) . ?
C181 H18C 0.97(2) . ?
C181 H18B 0.98(2) . ?
C181 H18A 1.01(2) . ?
C182 H18F 0.97(2) . ?
C182 H18E 0.97(2) . ?
C182 H18D 0.95(2) . ?
C183 H18I 0.95(2) . ?
C183 H18H 0.99(2) . ?
C183 H18G 0.95(2) . ?
C271 H27C 0.933(19) . ?
C271 H27B 0.96(2) . ?
C271 H27A 0.95(2) . ?
C272 H27F 0.963(18) . ?
C272 H27E 0.940(19) . ?
C272 H27D 0.928(19) . ?
C273 H27I 0.958(19) . ?
C273 H27H 0.95(2) . ?
C273 H27G 0.98(2) . ?
C281 H28C 0.94(2) . ?
C281 H28B 0.94(2) . ?
C281 H28A 0.98(2) . ?
C282 H28F 0.97(2) . ?
C282 H28E 0.95(2) . ?
C282 H28D 1.02(2) . ?
C283 H28I 1.01(2) . ?
C283 H28H 0.97(2) . ?
C283 H28G 1.01(2) . ?
