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#$Date: 2025-10-04 21:44:59 +0300 (Sat, 04 Oct 2025) $
#$Revision: 302373 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/95/7719553.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_7719553
loop_
_publ_author_name
'Wang, Lei'
'Wang, Li-Xin'
'Liu, Zhao-Long'
'Xu, Fang'
'Qi, Rui-Yue'
'Man, Wai-Lun'
'Xiang, Jing'
'Liu, Ji-Yan'
'Lau, Tai-Chu'
_publ_section_title
;
 Reaction of an osmium(VI) nitrido complex with enamines generated in
 situ from ketones and anilines.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14052
_journal_page_last               14058
_journal_paper_doi               10.1039/d5dt01334h
_journal_volume                  54
_journal_year                    2025
_chemical_formula_sum            'C53.5 H43 N8 O5 Os P'
_chemical_formula_weight         1099.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2023-11-16 deposited with the CCDC.	2025-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.161(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3204(3)
_cell_length_b                   16.0179(4)
_cell_length_c                   23.9832(8)
_cell_measurement_reflns_used    9328
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      74.55
_cell_measurement_theta_min      3.35
_cell_volume                     4982.8(2)
_computing_cell_refinement       'Bruker Saint'
_computing_data_collection       'Bruker Apex3'
_computing_data_reduction        'Bruker Saint'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture Photon II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            65163
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.543
_diffrn_reflns_theta_min         3.346
_diffrn_source                   'micro focus'
_exptl_absorpt_coefficient_mu    5.589
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.6023
_exptl_absorpt_correction_type   multi-scan
_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            purple
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_description       block
_exptl_crystal_F_000             2204
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.407
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     620
_refine_ls_number_reflns         10171
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0285
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0385P)²+3.9887P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_refine_ls_wR_factor_ref         0.0722
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9183
_reflns_number_total             10171
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5dt01334h2.cif
_cod_data_source_block           1_a_CCDC1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C53.50 H43 N8 O5 Os P'
_cod_database_code               7719553
_shelx_shelxl_version_number     2016/6
_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_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
Os1 Os 0.26084(2) 0.56227(2) 0.55756(2) 0.02072(5) Uani 1 1 d . . . . .
O1 O 0.39479(14) 0.50564(12) 0.54926(8) 0.0257(4) Uani 1 1 d . . . . .
O2 O 0.34064(18) 0.39680(13) 0.69910(9) 0.0359(4) Uani 1 1 d . . . . .
O3 O 0.8140(2) 0.4362(2) 0.71767(12) 0.0615(8) Uani 1 1 d . . . . .
O4 O 0.7129(2) 0.4044(2) 0.77295(10) 0.0562(7) Uani 1 1 d . . . . .
N1 N 0.12805(17) 0.61769(14) 0.56815(10) 0.0254(4) Uani 1 1 d D . . . .
H1 H 0.077(2) 0.624(2) 0.5387(11) 0.030 Uiso 1 1 d D U . . .
N2 N 0.1754(2) 0.66549(17) 0.66167(10) 0.0342(5) Uani 1 1 d . . . . .
H2 H 0.239567 0.669155 0.658050 0.041 Uiso 1 1 calc R U . . .
N3 N 0.00416(18) 0.67830(16) 0.60885(11) 0.0326(5) Uani 1 1 d . . . . .
H3 H -0.044312 0.641659 0.594956 0.039 Uiso 1 1 calc R U . . .
N4 N 0.1207(2) 0.42884(17) 0.47529(13) 0.0409(6) Uani 1 1 d . . . . .
N5 N 0.25197(19) 0.67699(17) 0.44891(11) 0.0348(5) Uani 1 1 d . . . . .
N6 N 0.4065(2) 0.69679(17) 0.63615(14) 0.0462(7) Uani 1 1 d . . . . .
N7 N 0.26724(18) 0.47991(13) 0.62682(9) 0.0258(4) Uani 1 1 d . . . . .
N8 N 0.7277(2) 0.4269(2) 0.72648(12) 0.0451(7) Uani 1 1 d . . . . .
C1 C 0.1039(2) 0.65378(16) 0.61253(12) 0.0265(5) Uani 1 1 d . . . . .
C2 C 0.1615(3) 0.67268(19) 0.71824(13) 0.0397(7) Uani 1 1 d . . . . .
C3 C 0.2351(4) 0.7182(3) 0.75708(16) 0.0606(11) Uani 1 1 d . . . . .
H3A H 0.290729 0.743928 0.744872 0.073 Uiso 1 1 calc R U . . .
C4 C 0.2272(6) 0.7260(3) 0.81331(18) 0.0816(17) Uani 1 1 d . . . . .
H4 H 0.277104 0.757654 0.839488 0.098 Uiso 1 1 calc R U . . .
C5 C 0.1490(5) 0.6890(4) 0.83137(19) 0.0790(16) Uani 1 1 d . . . . .
H5 H 0.144235 0.694669 0.870112 0.095 Uiso 1 1 calc R U . . .
C6 C 0.0765(5) 0.6431(4) 0.7938(2) 0.0783(16) Uani 1 1 d . . . . .
H6 H 0.021759 0.617320 0.806805 0.094 Uiso 1 1 calc R U . . .
C7 C 0.0822(3) 0.6338(3) 0.73618(17) 0.0562(9) Uani 1 1 d . . . . .
H7 H 0.032601 0.601459 0.710346 0.067 Uiso 1 1 calc R U . . .
C8 C -0.0285(2) 0.75633(19) 0.62509(12) 0.0331(6) Uani 1 1 d . . . . .
C9 C 0.0378(3) 0.8220(2) 0.64637(14) 0.0404(7) Uani 1 1 d . . . . .
H9 H 0.110341 0.814237 0.654327 0.048 Uiso 1 1 calc R U . . .
C10 C -0.0037(4) 0.8994(2) 0.65587(16) 0.0531(9) Uani 1 1 d . . . . .
H10 H 0.041432 0.944021 0.670834 0.064 Uiso 1 1 calc R U . . .
C11 C -0.1075(4) 0.9123(3) 0.64411(18) 0.0652(12) Uani 1 1 d . . . . .
H11 H -0.134101 0.965962 0.649422 0.078 Uiso 1 1 calc R U . . .
C12 C -0.1742(3) 0.8468(3) 0.62438(17) 0.0610(11) Uani 1 1 d . . . . .
H12 H -0.246615 0.855083 0.617054 0.073 Uiso 1 1 calc R U . . .
C13 C -0.1344(3) 0.7689(3) 0.61537(15) 0.0458(8) Uani 1 1 d . . . . .
H13 H -0.180099 0.723764 0.602443 0.055 Uiso 1 1 calc R U . . .
C14 C 0.1709(2) 0.47687(17) 0.50408(12) 0.0272(5) Uani 1 1 d . . . . .
C15 C 0.25703(19) 0.63500(17) 0.48801(12) 0.0263(5) Uani 1 1 d . . . . .
C16 C 0.3549(2) 0.64749(17) 0.60889(12) 0.0279(5) Uani 1 1 d . . . . .
C17 C 0.4699(2) 0.48623(16) 0.59242(11) 0.0243(5) Uani 1 1 d . . . . .
C18 C 0.5713(2) 0.48574(18) 0.58328(12) 0.0302(5) Uani 1 1 d . . . . .
H18 H 0.581627 0.499354 0.546446 0.036 Uiso 1 1 calc R U . . .
C19 C 0.6548(2) 0.4661(2) 0.62631(12) 0.0330(6) Uani 1 1 d . . . . .
H19 H 0.722359 0.467201 0.619624 0.040 Uiso 1 1 calc R U . . .
C20 C 0.6391(2) 0.44437(19) 0.68032(13) 0.0340(6) Uani 1 1 d . . . . .
C21 C 0.5414(2) 0.43951(18) 0.69063(13) 0.0329(6) Uani 1 1 d . . . . .
H21 H 0.532255 0.421983 0.726994 0.040 Uiso 1 1 calc R U . . .
C22 C 0.4561(2) 0.46052(17) 0.64722(12) 0.0279(5) Uani 1 1 d . . . . .
C23 C 0.3537(2) 0.44956(16) 0.65686(11) 0.0274(5) Uani 1 1 d . . . . .
C24 C 0.2352(3) 0.39317(19) 0.69388(13) 0.0357(6) Uani 1 1 d . . . . .
C25 C 0.1815(3) 0.3473(2) 0.72663(16) 0.0472(8) Uani 1 1 d . . . . .
H25 H 0.215499 0.313768 0.757920 0.057 Uiso 1 1 calc R U . . .
C26 C 0.0754(3) 0.3537(2) 0.71074(17) 0.0511(9) Uani 1 1 d . . . . .
H26 H 0.034933 0.324150 0.732063 0.061 Uiso 1 1 calc R U . . .
C27 C 0.0264(3) 0.4019(2) 0.66468(16) 0.0441(8) Uani 1 1 d . . . . .
H27 H -0.046793 0.403586 0.654927 0.053 Uiso 1 1 calc R U . . .
C28 C 0.0809(2) 0.44808(18) 0.63213(15) 0.0353(6) Uani 1 1 d . . . . .
H28 H 0.046904 0.481063 0.600523 0.042 Uiso 1 1 calc R U . . .
C29 C 0.1881(2) 0.44318(16) 0.64850(13) 0.0300(6) Uani 1 1 d . . . . .
P1 P 0.73332(5) 0.63774(4) 0.91576(3) 0.03022(14) Uani 1 1 d . . . . .
C30 C 0.7087(3) 0.64949(19) 0.83910(14) 0.0399(7) Uani 1 1 d . . . . .
C31 C 0.7824(3) 0.6238(2) 0.81041(16) 0.0489(8) Uani 1 1 d . . . . .
H31 H 0.847372 0.603852 0.831065 0.059 Uiso 1 1 calc R U . . .
C32 C 0.7599(4) 0.6277(3) 0.75078(17) 0.0644(12) Uani 1 1 d . . . . .
H32 H 0.810231 0.610392 0.730757 0.077 Uiso 1 1 calc R U . . .
C33 C 0.6665(5) 0.6561(3) 0.72083(19) 0.0769(17) Uani 1 1 d . . . . .
H33 H 0.651399 0.657325 0.680169 0.092 Uiso 1 1 calc R U . . .
C34 C 0.5944(5) 0.6830(4) 0.7497(2) 0.0808(16) Uani 1 1 d . . . . .
H34 H 0.529606 0.703070 0.728760 0.097 Uiso 1 1 calc R U . . .
C35 C 0.6152(3) 0.6810(3) 0.80858(19) 0.0633(11) Uani 1 1 d . . . . .
H35 H 0.565752 0.701042 0.828270 0.076 Uiso 1 1 calc R U . . .
C36 C 0.8664(2) 0.66090(17) 0.94447(12) 0.0288(5) Uani 1 1 d . . . . .
C37 C 0.9096(2) 0.73200(18) 0.92528(13) 0.0344(6) Uani 1 1 d . . . . .
H37 H 0.868833 0.766788 0.896824 0.041 Uiso 1 1 calc R U . . .
C38 C 1.0120(2) 0.75133(19) 0.94802(14) 0.0366(6) Uani 1 1 d . . . . .
H38 H 1.041439 0.799975 0.935593 0.044 Uiso 1 1 calc R U . . .
C39 C 1.0716(2) 0.6999(2) 0.98880(14) 0.0384(6) Uani 1 1 d . . . . .
H39 H 1.142069 0.712900 1.003957 0.046 Uiso 1 1 calc R U . . .
C40 C 1.0289(3) 0.6294(2) 1.00765(14) 0.0400(7) Uani 1 1 d . . . . .
H40 H 1.070330 0.594618 1.035835 0.048 Uiso 1 1 calc R U . . .
C41 C 0.9263(2) 0.60928(18) 0.98576(13) 0.0339(6) Uani 1 1 d . . . . .
H41 H 0.897246 0.560898 0.998737 0.041 Uiso 1 1 calc R U . . .
C42 C 0.6532(2) 0.70589(18) 0.94566(14) 0.0350(6) Uani 1 1 d . . . . .
C43 C 0.6949(2) 0.77504(18) 0.97765(14) 0.0342(6) Uani 1 1 d . . . . .
H43 H 0.766483 0.786835 0.983852 0.041 Uiso 1 1 calc R U . . .
C44 C 0.6306(3) 0.82673(19) 1.00047(16) 0.0413(7) Uani 1 1 d . . . . .
H44 H 0.658957 0.873143 1.023378 0.050 Uiso 1 1 calc R U . . .
C45 C 0.5258(3) 0.8113(2) 0.99017(17) 0.0444(7) Uani 1 1 d . . . . .
H45 H 0.482437 0.847394 1.005603 0.053 Uiso 1 1 calc R U . . .
C46 C 0.4840(3) 0.7431(2) 0.95735(18) 0.0477(8) Uani 1 1 d . . . . .
H46 H 0.411716 0.733526 0.949408 0.057 Uiso 1 1 calc R U . . .
C47 C 0.5471(3) 0.6891(2) 0.93616(17) 0.0452(7) Uani 1 1 d . . . . .
H47 H 0.518992 0.640930 0.915272 0.054 Uiso 1 1 calc R U . . .
C48 C 0.7066(2) 0.53219(18) 0.93325(13) 0.0339(6) Uani 1 1 d . . . . .
C49 C 0.6880(3) 0.5146(2) 0.98658(16) 0.0486(8) Uani 1 1 d . . . . .
H49 H 0.686065 0.558329 1.013075 0.058 Uiso 1 1 calc R U . . .
C50 C 0.6722(4) 0.4323(2) 1.00091(19) 0.0568(10) Uani 1 1 d . . . . .
H50 H 0.660361 0.419510 1.037544 0.068 Uiso 1 1 calc R U . . .
C51 C 0.6738(3) 0.3690(2) 0.96176(18) 0.0500(8) Uani 1 1 d . . . . .
H51 H 0.661893 0.312881 0.971408 0.060 Uiso 1 1 calc R U . . .
C52 C 0.6925(3) 0.3868(2) 0.90937(17) 0.0452(8) Uani 1 1 d . . . . .
H52 H 0.693949 0.342954 0.882916 0.054 Uiso 1 1 calc R U . . .
C53 C 0.7096(3) 0.4687(2) 0.89432(15) 0.0395(7) Uani 1 1 d . . . . .
H53 H 0.723028 0.480853 0.857951 0.047 Uiso 1 1 calc R U . . .
O5 O 0.4169(6) 0.4945(5) 0.8840(4) 0.084(2) Uiso 0.5 1 d . . P . .
H5A H 0.423465 0.441749 0.885964 0.100 Uiso 0.5 1 d R U P . .
C54 C 0.3739(10) 0.5133(8) 0.8258(6) 0.087(3) Uiso 0.5 1 d . . P . .
H54A H 0.415950 0.555899 0.812566 0.130 Uiso 0.5 1 calc R U P . .
H54B H 0.303512 0.534413 0.821776 0.130 Uiso 0.5 1 calc R U P . .
H54C H 0.372285 0.462688 0.802645 0.130 Uiso 0.5 1 calc R U P . .
O6 O -0.4356(5) 0.8169(4) 0.6107(3) 0.0687(16) Uiso 0.5 1 d . . P . .
H6A H -0.489459 0.798640 0.619943 0.082 Uiso 0.5 1 d R U P . .
H6B H -0.431447 0.804690 0.576784 0.082 Uiso 0.5 1 d R U P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -4.9801 6.2216 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 '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
C15 Os1 N1 89.57(10) . . ?
C15 Os1 O1 91.93(9) . . ?
N1 Os1 O1 178.41(8) . . ?
C15 Os1 C16 90.51(11) . . ?
N1 Os1 C16 93.67(10) . . ?
O1 Os1 C16 85.79(9) . . ?
C15 Os1 C14 88.12(11) . . ?
N1 Os1 C14 88.20(10) . . ?
O1 Os1 C14 92.38(9) . . ?
C16 Os1 C14 177.67(11) . . ?
C15 Os1 N7 176.23(9) . . ?
N1 Os1 N7 93.13(9) . . ?
O1 Os1 N7 85.39(8) . . ?
C16 Os1 N7 91.94(10) . . ?
C14 Os1 N7 89.34(10) . . ?
C17 O1 Os1 123.79(16) . . ?
C23 O2 C24 105.0(2) . . ?
C1 N1 Os1 132.05(18) . . ?
C1 N1 H1 108(2) . . ?
Os1 N1 H1 119(2) . . ?
C1 N2 C2 128.9(3) . . ?
C1 N2 H2 115.6 . . ?
C2 N2 H2 115.6 . . ?
C1 N3 C8 126.4(2) . . ?
C1 N3 H3 116.8 . . ?
C8 N3 H3 116.8 . . ?
C23 N7 C29 106.4(2) . . ?
C23 N7 Os1 122.70(19) . . ?
C29 N7 Os1 130.85(19) . . ?
O3 N8 O4 122.9(3) . . ?
O3 N8 C20 118.5(3) . . ?
O4 N8 C20 118.6(3) . . ?
N1 C1 N2 120.9(2) . . ?
N1 C1 N3 119.2(2) . . ?
N2 C1 N3 119.9(2) . . ?
C7 C2 C3 120.0(4) . . ?
C7 C2 N2 122.7(3) . . ?
C3 C2 N2 117.2(3) . . ?
C4 C3 C2 120.0(5) . . ?
C4 C3 H3A 120.0 . . ?
C2 C3 H3A 120.0 . . ?
C5 C4 C3 120.5(5) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
C4 C5 C6 120.1(4) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C5 C6 C7 120.8(5) . . ?
C5 C6 H6 119.6 . . ?
C7 C6 H6 119.6 . . ?
C2 C7 C6 118.4(5) . . ?
C2 C7 H7 120.8 . . ?
C6 C7 H7 120.8 . . ?
C13 C8 C9 119.1(3) . . ?
C13 C8 N3 116.6(3) . . ?
C9 C8 N3 124.2(3) . . ?
C8 C9 C10 119.3(3) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
C11 C10 C9 121.4(4) . . ?
C11 C10 H10 119.3 . . ?
C9 C10 H10 119.3 . . ?
C10 C11 C12 119.9(4) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C11 C12 C13 119.6(4) . . ?
C11 C12 H12 120.2 . . ?
C13 C12 H12 120.2 . . ?
C8 C13 C12 120.7(4) . . ?
C8 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
N4 C14 Os1 178.8(3) . . ?
N5 C15 Os1 177.9(2) . . ?
N6 C16 Os1 177.9(3) . . ?
O1 C17 C18 117.7(2) . . ?
O1 C17 C22 124.3(2) . . ?
C18 C17 C22 117.9(2) . . ?
C19 C18 C17 121.6(3) . . ?
C19 C18 H18 119.2 . . ?
C17 C18 H18 119.2 . . ?
C18 C19 C20 119.1(3) . . ?
C18 C19 H19 120.4 . . ?
C20 C19 H19 120.4 . . ?
C21 C20 C19 121.6(3) . . ?
C21 C20 N8 119.3(3) . . ?
C19 C20 N8 119.2(3) . . ?
C20 C21 C22 119.5(3) . . ?
C20 C21 H21 120.2 . . ?
C22 C21 H21 120.2 . . ?
C21 C22 C17 120.1(3) . . ?
C21 C22 C23 119.3(3) . . ?
C17 C22 C23 120.4(2) . . ?
N7 C23 O2 113.3(3) . . ?
N7 C23 C22 127.8(2) . . ?
O2 C23 C22 118.7(2) . . ?
C29 C24 O2 108.4(2) . . ?
C29 C24 C25 123.6(3) . . ?
O2 C24 C25 127.9(3) . . ?
C26 C25 C24 115.6(3) . . ?
C26 C25 H25 122.2 . . ?
C24 C25 H25 122.2 . . ?
C25 C26 C27 121.9(3) . . ?
C25 C26 H26 119.0 . . ?
C27 C26 H26 119.0 . . ?
C26 C27 C28 122.2(3) . . ?
C26 C27 H27 118.9 . . ?
C28 C27 H27 118.9 . . ?
C27 C28 C29 116.3(3) . . ?
C27 C28 H28 121.8 . . ?
C29 C28 H28 121.8 . . ?
C24 C29 C28 120.4(3) . . ?
C24 C29 N7 106.9(3) . . ?
C28 C29 N7 132.7(3) . . ?
C42 P1 C36 110.43(14) . . ?
C42 P1 C48 108.21(15) . . ?
C36 P1 C48 109.70(14) . . ?
C42 P1 C30 111.04(16) . . ?
C36 P1 C30 107.78(15) . . ?
C48 P1 C30 109.68(14) . . ?
C31 C30 C35 119.9(4) . . ?
C31 C30 P1 119.4(3) . . ?
C35 C30 P1 120.6(3) . . ?
C30 C31 C32 119.1(4) . . ?
C30 C31 H31 120.4 . . ?
C32 C31 H31 120.4 . . ?
C33 C32 C31 120.7(5) . . ?
C33 C32 H32 119.6 . . ?
C31 C32 H32 119.6 . . ?
C32 C33 C34 119.8(4) . . ?
C32 C33 H33 120.1 . . ?
C34 C33 H33 120.1 . . ?
C33 C34 C35 120.6(5) . . ?
C33 C34 H34 119.7 . . ?
C35 C34 H34 119.7 . . ?
C34 C35 C30 119.8(5) . . ?
C34 C35 H35 120.1 . . ?
C30 C35 H35 120.1 . . ?
C41 C36 C37 120.3(3) . . ?
C41 C36 P1 120.5(2) . . ?
C37 C36 P1 119.2(2) . . ?
C38 C37 C36 119.6(3) . . ?
C38 C37 H37 120.2 . . ?
C36 C37 H37 120.2 . . ?
C39 C38 C37 120.0(3) . . ?
C39 C38 H38 120.0 . . ?
C37 C38 H38 120.0 . . ?
C38 C39 C40 120.3(3) . . ?
C38 C39 H39 119.8 . . ?
C40 C39 H39 119.8 . . ?
C39 C40 C41 120.6(3) . . ?
C39 C40 H40 119.7 . . ?
C41 C40 H40 119.7 . . ?
C40 C41 C36 119.1(3) . . ?
C40 C41 H41 120.4 . . ?
C36 C41 H41 120.4 . . ?
C43 C42 C47 120.2(3) . . ?
C43 C42 P1 120.5(2) . . ?
C47 C42 P1 119.3(2) . . ?
C42 C43 C44 119.2(3) . . ?
C42 C43 H43 120.4 . . ?
C44 C43 H43 120.4 . . ?
C45 C44 C43 120.7(3) . . ?
C45 C44 H44 119.7 . . ?
C43 C44 H44 119.7 . . ?
C44 C45 C46 120.1(3) . . ?
C44 C45 H45 120.0 . . ?
C46 C45 H45 120.0 . . ?
C47 C46 C45 120.1(3) . . ?
C47 C46 H46 119.9 . . ?
C45 C46 H46 119.9 . . ?
C46 C47 C42 119.7(3) . . ?
C46 C47 H47 120.2 . . ?
C42 C47 H47 120.2 . . ?
C49 C48 C53 120.7(3) . . ?
C49 C48 P1 119.6(2) . . ?
C53 C48 P1 119.7(2) . . ?
C48 C49 C50 119.3(3) . . ?
C48 C49 H49 120.3 . . ?
C50 C49 H49 120.3 . . ?
C51 C50 C49 120.0(4) . . ?
C51 C50 H50 120.0 . . ?
C49 C50 H50 120.0 . . ?
C52 C51 C50 120.2(3) . . ?
C52 C51 H51 119.9 . . ?
C50 C51 H51 119.9 . . ?
C51 C52 C53 120.7(3) . . ?
C51 C52 H52 119.6 . . ?
C53 C52 H52 119.6 . . ?
C48 C53 C52 119.0(3) . . ?
C48 C53 H53 120.5 . . ?
C52 C53 H53 120.5 . . ?
C54 O5 H5A 106.3 . . ?
O5 C54 H54A 109.5 . . ?
O5 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
O5 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
H6A O6 H6B 114.4 . . ?
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 C15 2.026(3) . ?
Os1 N1 2.046(2) . ?
Os1 O1 2.0513(18) . ?
Os1 C16 2.061(3) . ?
Os1 C14 2.062(3) . ?
Os1 N7 2.108(2) . ?
O1 C17 1.303(3) . ?
O2 C23 1.361(3) . ?
O2 C24 1.383(4) . ?
O3 N8 1.224(5) . ?
O4 N8 1.229(4) . ?
N1 C1 1.314(4) . ?
N1 H1 0.870(18) . ?
N2 C1 1.350(4) . ?
N2 C2 1.415(4) . ?
N2 H2 0.8800 . ?
N3 C1 1.368(4) . ?
N3 C8 1.407(4) . ?
N3 H3 0.8800 . ?
N4 C14 1.142(4) . ?
N5 C15 1.144(4) . ?
N6 C16 1.148(4) . ?
N7 C23 1.305(4) . ?
N7 C29 1.406(4) . ?
N8 C20 1.449(4) . ?
C2 C7 1.376(6) . ?
C2 C3 1.395(5) . ?
C3 C4 1.382(6) . ?
C3 H3A 0.9500 . ?
C4 C5 1.353(10) . ?
C4 H4 0.9500 . ?
C5 C6 1.375(9) . ?
C5 H5 0.9500 . ?
C6 C7 1.409(6) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C13 1.391(5) . ?
C8 C9 1.394(5) . ?
C9 C10 1.397(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.362(7) . ?
C10 H10 0.9500 . ?
C11 C12 1.386(8) . ?
C11 H11 0.9500 . ?
C12 C13 1.392(5) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C17 C18 1.416(4) . ?
C17 C22 1.429(4) . ?
C18 C19 1.371(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.402(4) . ?
C19 H19 0.9500 . ?
C20 C21 1.382(5) . ?
C21 C22 1.396(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.445(4) . ?
C24 C29 1.382(5) . ?
C24 C25 1.386(5) . ?
C25 C26 1.381(6) . ?
C25 H25 0.9500 . ?
C26 C27 1.384(6) . ?
C26 H26 0.9500 . ?
C27 C28 1.393(5) . ?
C27 H27 0.9500 . ?
C28 C29 1.394(5) . ?
C28 H28 0.9500 . ?
P1 C42 1.787(3) . ?
P1 C36 1.789(3) . ?
P1 C48 1.797(3) . ?
P1 C30 1.802(3) . ?
C30 C31 1.383(6) . ?
C30 C35 1.387(6) . ?
C31 C32 1.394(6) . ?
C31 H31 0.9500 . ?
C32 C33 1.366(8) . ?
C32 H32 0.9500 . ?
C33 C34 1.374(10) . ?
C33 H33 0.9500 . ?
C34 C35 1.377(7) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 C41 1.393(4) . ?
C36 C37 1.400(4) . ?
C37 C38 1.384(4) . ?
C37 H37 0.9500 . ?
C38 C39 1.383(5) . ?
C38 H38 0.9500 . ?
C39 C40 1.385(5) . ?
C39 H39 0.9500 . ?
C40 C41 1.386(5) . ?
C40 H40 0.9500 . ?
C41 H41 0.9500 . ?
C42 C43 1.389(4) . ?
C42 C47 1.404(4) . ?
C43 C44 1.390(5) . ?
C43 H43 0.9500 . ?
C44 C45 1.384(5) . ?
C44 H44 0.9500 . ?
C45 C46 1.386(5) . ?
C45 H45 0.9500 . ?
C46 C47 1.382(5) . ?
C46 H46 0.9500 . ?
C47 H47 0.9500 . ?
C48 C49 1.386(5) . ?
C48 C53 1.388(4) . ?
C49 C50 1.390(5) . ?
C49 H49 0.9500 . ?
C50 C51 1.386(6) . ?
C50 H50 0.9500 . ?
C51 C52 1.366(6) . ?
C51 H51 0.9500 . ?
C52 C53 1.392(5) . ?
C52 H52 0.9500 . ?
C53 H53 0.9500 . ?
O5 C54 1.415(15) . ?
O5 H5A 0.8500 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
O6 H6A 0.8500 . ?
O6 H6B 0.8500 . ?
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
Os1 N1 C1 N2 5.6(4) . . . . ?
Os1 N1 C1 N3 -173.3(2) . . . . ?
C2 N2 C1 N1 -153.9(3) . . . . ?
C2 N2 C1 N3 25.0(5) . . . . ?
C8 N3 C1 N1 -132.4(3) . . . . ?
C8 N3 C1 N2 48.8(4) . . . . ?
C1 N2 C2 C7 29.8(5) . . . . ?
C1 N2 C2 C3 -153.3(3) . . . . ?
C7 C2 C3 C4 -1.5(6) . . . . ?
N2 C2 C3 C4 -178.5(4) . . . . ?
C2 C3 C4 C5 0.7(8) . . . . ?
C3 C4 C5 C6 0.0(8) . . . . ?
C4 C5 C6 C7 0.1(8) . . . . ?
C3 C2 C7 C6 1.6(6) . . . . ?
N2 C2 C7 C6 178.4(4) . . . . ?
C5 C6 C7 C2 -0.9(7) . . . . ?
C1 N3 C8 C13 177.5(3) . . . . ?
C1 N3 C8 C9 1.8(5) . . . . ?
C13 C8 C9 C10 -1.8(5) . . . . ?
N3 C8 C9 C10 173.8(3) . . . . ?
C8 C9 C10 C11 -0.8(6) . . . . ?
C9 C10 C11 C12 2.5(7) . . . . ?
C10 C11 C12 C13 -1.6(7) . . . . ?
C9 C8 C13 C12 2.7(5) . . . . ?
N3 C8 C13 C12 -173.2(3) . . . . ?
C11 C12 C13 C8 -1.0(6) . . . . ?
Os1 O1 C17 C18 -150.40(19) . . . . ?
Os1 O1 C17 C22 33.6(3) . . . . ?
O1 C17 C18 C19 180.0(3) . . . . ?
C22 C17 C18 C19 -3.8(4) . . . . ?
C17 C18 C19 C20 1.3(5) . . . . ?
C18 C19 C20 C21 2.3(5) . . . . ?
C18 C19 C20 N8 -177.5(3) . . . . ?
O3 N8 C20 C21 -175.8(3) . . . . ?
O4 N8 C20 C21 3.4(5) . . . . ?
O3 N8 C20 C19 4.0(5) . . . . ?
O4 N8 C20 C19 -176.9(3) . . . . ?
C19 C20 C21 C22 -3.1(4) . . . . ?
N8 C20 C21 C22 176.6(3) . . . . ?
C20 C21 C22 C17 0.5(4) . . . . ?
C20 C21 C22 C23 175.6(3) . . . . ?
O1 C17 C22 C21 178.9(3) . . . . ?
C18 C17 C22 C21 2.9(4) . . . . ?
O1 C17 C22 C23 3.9(4) . . . . ?
C18 C17 C22 C23 -172.1(2) . . . . ?
C29 N7 C23 O2 -2.2(3) . . . . ?
Os1 N7 C23 O2 -179.18(17) . . . . ?
C29 N7 C23 C22 172.5(3) . . . . ?
Os1 N7 C23 C22 -4.5(4) . . . . ?
C24 O2 C23 N7 1.1(3) . . . . ?
C24 O2 C23 C22 -174.1(2) . . . . ?
C21 C22 C23 N7 165.6(3) . . . . ?
C17 C22 C23 N7 -19.4(4) . . . . ?
C21 C22 C23 O2 -19.9(4) . . . . ?
C17 C22 C23 O2 155.1(2) . . . . ?
C23 O2 C24 C29 0.5(3) . . . . ?
C23 O2 C24 C25 179.5(3) . . . . ?
C29 C24 C25 C26 0.7(5) . . . . ?
O2 C24 C25 C26 -178.2(3) . . . . ?
C24 C25 C26 C27 0.8(5) . . . . ?
C25 C26 C27 C28 -1.1(5) . . . . ?
C26 C27 C28 C29 0.0(5) . . . . ?
O2 C24 C29 C28 177.2(3) . . . . ?
C25 C24 C29 C28 -1.8(5) . . . . ?
O2 C24 C29 N7 -1.8(3) . . . . ?
C25 C24 C29 N7 179.2(3) . . . . ?
C27 C28 C29 C24 1.4(4) . . . . ?
C27 C28 C29 N7 -179.9(3) . . . . ?
C23 N7 C29 C24 2.4(3) . . . . ?
Os1 N7 C29 C24 179.01(19) . . . . ?
C23 N7 C29 C28 -176.4(3) . . . . ?
Os1 N7 C29 C28 0.2(5) . . . . ?
C42 P1 C30 C31 159.4(3) . . . . ?
C36 P1 C30 C31 38.4(3) . . . . ?
C48 P1 C30 C31 -81.0(3) . . . . ?
C42 P1 C30 C35 -23.1(4) . . . . ?
C36 P1 C30 C35 -144.1(3) . . . . ?
C48 P1 C30 C35 96.5(3) . . . . ?
C35 C30 C31 C32 -2.0(5) . . . . ?
P1 C30 C31 C32 175.6(3) . . . . ?
C30 C31 C32 C33 -0.2(6) . . . . ?
C31 C32 C33 C34 1.4(7) . . . . ?
C32 C33 C34 C35 -0.4(8) . . . . ?
C33 C34 C35 C30 -1.7(8) . . . . ?
C31 C30 C35 C34 2.9(7) . . . . ?
P1 C30 C35 C34 -174.6(4) . . . . ?
C42 P1 C36 C41 104.2(3) . . . . ?
C48 P1 C36 C41 -15.0(3) . . . . ?
C30 P1 C36 C41 -134.4(2) . . . . ?
C42 P1 C36 C37 -75.3(3) . . . . ?
C48 P1 C36 C37 165.5(2) . . . . ?
C30 P1 C36 C37 46.1(3) . . . . ?
C41 C36 C37 C38 -0.7(5) . . . . ?
P1 C36 C37 C38 178.8(2) . . . . ?
C36 C37 C38 C39 1.0(5) . . . . ?
C37 C38 C39 C40 -0.8(5) . . . . ?
C38 C39 C40 C41 0.3(5) . . . . ?
C39 C40 C41 C36 0.0(5) . . . . ?
C37 C36 C41 C40 0.2(5) . . . . ?
P1 C36 C41 C40 -179.3(2) . . . . ?
C36 P1 C42 C43 11.0(3) . . . . ?
C48 P1 C42 C43 131.1(3) . . . . ?
C30 P1 C42 C43 -108.5(3) . . . . ?
C36 P1 C42 C47 -169.4(3) . . . . ?
C48 P1 C42 C47 -49.3(3) . . . . ?
C30 P1 C42 C47 71.1(3) . . . . ?
C47 C42 C43 C44 0.6(5) . . . . ?
P1 C42 C43 C44 -179.8(3) . . . . ?
C42 C43 C44 C45 -1.9(5) . . . . ?
C43 C44 C45 C46 0.8(5) . . . . ?
C44 C45 C46 C47 1.8(6) . . . . ?
C45 C46 C47 C42 -3.1(6) . . . . ?
C43 C42 C47 C46 1.9(5) . . . . ?
P1 C42 C47 C46 -177.7(3) . . . . ?
C42 P1 C48 C49 -38.3(3) . . . . ?
C36 P1 C48 C49 82.3(3) . . . . ?
C30 P1 C48 C49 -159.5(3) . . . . ?
C42 P1 C48 C53 144.8(3) . . . . ?
C36 P1 C48 C53 -94.7(3) . . . . ?
C30 P1 C48 C53 23.5(3) . . . . ?
C53 C48 C49 C50 0.0(6) . . . . ?
P1 C48 C49 C50 -176.9(3) . . . . ?
C48 C49 C50 C51 -0.8(7) . . . . ?
C49 C50 C51 C52 1.1(7) . . . . ?
C50 C51 C52 C53 -0.4(6) . . . . ?
C49 C48 C53 C52 0.7(5) . . . . ?
P1 C48 C53 C52 177.6(3) . . . . ?
C51 C52 C53 C48 -0.4(5) . . . . ?
