#------------------------------------------------------------------------------
#$Date: 2016-03-21 16:59:14 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178763 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/17/4101792.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_4101792
loop_
_publ_author_name
'Ruth Castro-Rodrigo'
'Miguel A. Esteruelas'
'Ana M. López'
'Fernando López'
'José L. Mascareñas'
'Montserrat Oliván'
'Enrique Oñate'
'Lucía Saya'
'Lara Villarino'
_publ_contact_author
;
  Dr. Enrique Oñate Rodríguez
  Departamento de Química Inorgánica - I.C.M.A.
  Facultad de Ciencias
  Universidad de Zaragoza - C.S.I.C.
  50009 Zaragoza, Spain
;
_publ_contact_author_email       enriqueo@posta.unizar.es
_publ_section_title
;
 Cleavage of Both C(sp3)-C(sp2) Bonds of Alkylidenecyclopropanes:
 Formation of Ethylene-Osmium-Vinylidene Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              454
_journal_page_last               455
_journal_paper_doi               10.1021/ja909240q
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C56 H71 B2 N6 O Os P'
_chemical_formula_weight         1086.98
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_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                92.519(2)
_cell_angle_beta                 96.857(2)
_cell_angle_gamma                118.8300(10)
_cell_formula_units_Z            2
_cell_length_a                   13.1940(12)
_cell_length_b                   13.2046(12)
_cell_length_c                   17.0692(15)
_cell_measurement_reflns_used    7345
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     2568.9(4)
_computing_cell_refinement       'SAINT+ v. 6.1 (Bruker AXS, 2000)'
_computing_data_collection       'SMART v. 5.625 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.1 (Bruker AXS, 2000)'
_computing_molecular_graphics    'XP, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       'ω rotations with narrow frames'
_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  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24537
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.74
_diffrn_reflns_theta_min         1.21
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    2.558
_exptl_absorpt_correction_T_max  0.822
_exptl_absorpt_correction_T_min  0.697
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Absorption correction performed with SADABS program. This is based on the
method of Blessing: Blessing, R. H., Acta Crystallogr., Sect. A 1995, 51, 33.

SADABS: Area-Detector Absorption Correction. Bruker-AXS 
within SAINT+ package, v. 6.1 (2000).
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1116
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.554
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         12077
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0345P)²+0.9614P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0770
_reflns_number_gt                10826
_reflns_number_total             12077
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja909240q_si_001_2.cif
_cod_data_source_block           mae363as
_cod_database_code               4101792
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Os Os 0.995558(11) 0.803964(11) 0.736141(7) 0.02058(4) Uani 1 1 d . . .
P P 1.18872(7) 0.94518(8) 0.70647(5) 0.02160(17) Uani 1 1 d . . .
O O 0.6465(2) 0.5367(2) 0.23080(15) 0.0371(6) Uani 1 1 d . . .
N1 N 0.8269(2) 0.6578(3) 0.74200(17) 0.0268(6) Uani 1 1 d . . .
N2 N 0.8067(2) 0.5470(2) 0.72810(16) 0.0254(6) Uani 1 1 d . . .
N3 N 0.9695(2) 0.6993(2) 0.62951(15) 0.0206(6) Uani 1 1 d . . .
N4 N 0.9388(2) 0.5850(2) 0.63066(15) 0.0215(6) Uani 1 1 d . . .
N5 N 1.0567(2) 0.6984(2) 0.80128(15) 0.0246(6) Uani 1 1 d . . .
N6 N 1.0088(2) 0.5828(2) 0.77313(15) 0.0247(6) Uani 1 1 d . . .
B1 B 0.9053(3) 0.5257(3) 0.7067(2) 0.0233(8) Uani 1 1 d . . .
H1 H 0.873(3) 0.434(3) 0.694(2) 0.028 Uiso 1 1 d . . .
B2 B 0.7884(3) 0.1472(3) 0.8563(2) 0.0189(7) Uani 1 1 d . . .
C1 C 0.9171(3) 0.8718(3) 0.6848(2) 0.0255(7) Uani 1 1 d . . .
C2 C 0.8444(3) 0.9061(3) 0.6539(2) 0.0328(8) Uani 1 1 d . . .
H2 H 0.865(4) 0.980(4) 0.670(2) 0.044(12) Uiso 1 1 d . . .
C3 C 0.7337(3) 0.8368(3) 0.5992(2) 0.0280(7) Uani 1 1 d . . .
C4 C 0.6589(3) 0.8830(4) 0.5831(2) 0.0332(8) Uani 1 1 d . . .
H4 H 0.6806 0.9584 0.6072 0.040 Uiso 1 1 calc R . .
C5 C 0.5535(4) 0.8198(4) 0.5322(2) 0.0431(10) Uani 1 1 d . . .
H5 H 0.5027 0.8515 0.5228 0.052 Uiso 1 1 calc R . .
C6 C 0.5210(4) 0.7112(4) 0.4949(3) 0.0505(11) Uani 1 1 d . . .
H6 H 0.4492 0.6688 0.4593 0.061 Uiso 1 1 calc R . .
C7 C 0.5951(4) 0.6655(4) 0.5105(3) 0.0478(11) Uani 1 1 d . . .
H7 H 0.5739 0.5909 0.4853 0.057 Uiso 1 1 calc R . .
C8 C 0.6998(3) 0.7271(3) 0.5625(2) 0.0376(9) Uani 1 1 d . . .
H8 H 0.7489 0.6937 0.5731 0.045 Uiso 1 1 calc R . .
C9 C 0.9517(5) 0.8501(4) 0.8489(3) 0.0444(11) Uani 1 1 d . . .
H9A H 0.891(4) 0.868(4) 0.831(2) 0.041(12) Uiso 1 1 d . . .
H9B H 0.936(4) 0.790(4) 0.877(3) 0.048(13) Uiso 1 1 d . . .
C10 C 1.0652(4) 0.9294(4) 0.8465(2) 0.0356(9) Uani 1 1 d . . .
H10A H 1.086(3) 1.006(3) 0.832(2) 0.029(10) Uiso 1 1 d . . .
H10B H 1.132(4) 0.924(4) 0.876(3) 0.051(13) Uiso 1 1 d . . .
C11 C 0.7239(3) 0.6499(4) 0.7513(2) 0.0362(9) Uani 1 1 d . . .
H11 H 0.7119 0.7143 0.7621 0.043 Uiso 1 1 calc R . .
C12 C 0.6375(3) 0.5340(4) 0.7428(2) 0.0395(10) Uani 1 1 d . . .
H12 H 0.5568 0.5040 0.7462 0.047 Uiso 1 1 calc R . .
C13 C 0.6932(3) 0.4722(3) 0.7285(2) 0.0322(8) Uani 1 1 d . . .
H13 H 0.6573 0.3898 0.7202 0.039 Uiso 1 1 calc R . .
C14 C 0.9651(3) 0.7178(3) 0.55274(18) 0.0246(7) Uani 1 1 d . . .
H14 H 0.9812 0.7900 0.5340 0.030 Uiso 1 1 calc R . .
C15 C 0.9337(3) 0.6167(3) 0.5049(2) 0.0299(8) Uani 1 1 d . . .
H15 H 0.9254 0.6061 0.4486 0.036 Uiso 1 1 calc R . .
C16 C 0.9173(3) 0.5354(3) 0.5560(2) 0.0284(7) Uani 1 1 d . . .
H16 H 0.8944 0.4562 0.5410 0.034 Uiso 1 1 calc R . .
C17 C 1.1296(3) 0.7160(3) 0.86883(19) 0.0300(8) Uani 1 1 d . . .
H17 H 1.1743 0.7883 0.9015 0.036 Uiso 1 1 calc R . .
C18 C 1.1307(3) 0.6152(3) 0.8843(2) 0.0322(8) Uani 1 1 d . . .
H18 H 1.1758 0.6047 0.9275 0.039 Uiso 1 1 calc R . .
C19 C 1.0525(3) 0.5329(3) 0.8237(2) 0.0278(7) Uani 1 1 d . . .
H19 H 1.0323 0.4532 0.8183 0.033 Uiso 1 1 calc R . .
C20 C 1.3136(3) 1.0220(3) 0.7904(2) 0.0341(9) Uani 1 1 d . . .
H20 H 1.2797 1.0360 0.8363 0.041 Uiso 1 1 calc R . .
C21 C 1.3679(3) 0.9471(4) 0.8177(2) 0.0428(10) Uani 1 1 d . . .
H21A H 1.4191 0.9471 0.7806 0.064 Uiso 1 1 calc R . .
H21B H 1.3054 0.8672 0.8189 0.064 Uiso 1 1 calc R . .
H21C H 1.4137 0.9791 0.8710 0.064 Uiso 1 1 calc R . .
C22 C 1.4116(3) 1.1412(4) 0.7771(3) 0.0454(11) Uani 1 1 d . . .
H22A H 1.4730 1.1732 0.8240 0.068 Uiso 1 1 calc R . .
H22B H 1.3796 1.1938 0.7683 0.068 Uiso 1 1 calc R . .
H22C H 1.4449 1.1329 0.7305 0.068 Uiso 1 1 calc R . .
C23 C 1.1916(3) 1.0699(3) 0.6582(2) 0.0283(7) Uani 1 1 d . . .
H23 H 1.2753 1.1227 0.6531 0.034 Uiso 1 1 calc R . .
C24 C 1.1565(3) 1.1413(3) 0.7099(2) 0.0358(9) Uani 1 1 d . . .
H24A H 1.1712 1.2124 0.6861 0.054 Uiso 1 1 calc R . .
H24B H 1.2028 1.1620 0.7632 0.054 Uiso 1 1 calc R . .
H24C H 1.0730 1.0954 0.7135 0.054 Uiso 1 1 calc R . .
C25 C 1.1226(3) 1.0383(3) 0.5740(2) 0.0346(8) Uani 1 1 d . . .
H25A H 1.0392 0.9867 0.5755 0.052 Uiso 1 1 calc R . .
H25B H 1.1512 0.9986 0.5406 0.052 Uiso 1 1 calc R . .
H25C H 1.1331 1.1094 0.5519 0.052 Uiso 1 1 calc R . .
C26 C 1.2396(3) 0.8801(3) 0.63261(19) 0.0273(7) Uani 1 1 d . . .
H26 H 1.1796 0.8552 0.5837 0.033 Uiso 1 1 calc R . .
C27 C 1.2405(3) 0.7681(3) 0.6534(2) 0.0346(9) Uani 1 1 d . . .
H27A H 1.2335 0.7219 0.6045 0.052 Uiso 1 1 calc R . .
H27B H 1.1743 0.7226 0.6809 0.052 Uiso 1 1 calc R . .
H27C H 1.3141 0.7886 0.6880 0.052 Uiso 1 1 calc R . .
C28 C 1.3564(3) 0.9639(3) 0.6063(2) 0.0363(9) Uani 1 1 d . . .
H28A H 1.4212 0.9832 0.6494 0.055 Uiso 1 1 calc R . .
H28B H 1.3558 1.0353 0.5935 0.055 Uiso 1 1 calc R . .
H28C H 1.3666 0.9267 0.5592 0.055 Uiso 1 1 calc R . .
C29 C 0.7145(3) 0.2010(3) 0.89720(17) 0.0184(6) Uani 1 1 d . . .
C30 C 0.6438(3) 0.1471(3) 0.95409(18) 0.0210(6) Uani 1 1 d . . .
H30 H 0.6348 0.0746 0.9678 0.025 Uiso 1 1 calc R . .
C31 C 0.5859(3) 0.1954(3) 0.99154(19) 0.0253(7) Uani 1 1 d . . .
H31 H 0.5389 0.1559 1.0300 0.030 Uiso 1 1 calc R . .
C32 C 0.5969(3) 0.3008(3) 0.97263(19) 0.0256(7) Uani 1 1 d . . .
H32 H 0.5574 0.3340 0.9976 0.031 Uiso 1 1 calc R . .
C33 C 0.6665(3) 0.3571(3) 0.91661(18) 0.0223(7) Uani 1 1 d . . .
H33 H 0.6743 0.4291 0.9027 0.027 Uiso 1 1 calc R . .
C34 C 0.7244(3) 0.3088(3) 0.88103(18) 0.0204(6) Uani 1 1 d . . .
H34 H 0.7732 0.3501 0.8439 0.025 Uiso 1 1 calc R . .
C35 C 0.7188(3) 0.0053(3) 0.85584(18) 0.0202(6) Uani 1 1 d . . .
C36 C 0.7286(3) -0.0498(3) 0.9225(2) 0.0264(7) Uani 1 1 d . . .
H36 H 0.7831 -0.0035 0.9683 0.032 Uiso 1 1 calc R . .
C37 C 0.6624(3) -0.1688(3) 0.9244(2) 0.0301(8) Uani 1 1 d . . .
H37 H 0.6718 -0.2021 0.9711 0.036 Uiso 1 1 calc R . .
C38 C 0.5830(3) -0.2390(3) 0.8591(2) 0.0340(8) Uani 1 1 d . . .
H38 H 0.5369 -0.3205 0.8605 0.041 Uiso 1 1 calc R . .
C39 C 0.5712(3) -0.1895(3) 0.7916(2) 0.0323(8) Uani 1 1 d . . .
H39 H 0.5174 -0.2371 0.7459 0.039 Uiso 1 1 calc R . .
C40 C 0.6380(3) -0.0700(3) 0.7904(2) 0.0274(7) Uani 1 1 d . . .
H40 H 0.6284 -0.0379 0.7432 0.033 Uiso 1 1 calc R . .
C41 C 0.9207(3) 0.2061(3) 0.90925(18) 0.0196(6) Uani 1 1 d . . .
C42 C 0.9753(3) 0.3149(3) 0.95374(18) 0.0225(7) Uani 1 1 d . . .
H42 H 0.9337 0.3568 0.9548 0.027 Uiso 1 1 calc R . .
C43 C 1.0877(3) 0.3651(3) 0.9966(2) 0.0277(7) Uani 1 1 d . . .
H43 H 1.1211 0.4398 1.0261 0.033 Uiso 1 1 calc R . .
C44 C 1.1509(3) 0.3075(3) 0.99667(19) 0.0267(7) Uani 1 1 d . . .
H44 H 1.2278 0.3415 1.0261 0.032 Uiso 1 1 calc R . .
C45 C 1.1010(3) 0.1995(3) 0.9534(2) 0.0303(8) Uani 1 1 d . . .
H45 H 1.1438 0.1588 0.9527 0.036 Uiso 1 1 calc R . .
C46 C 0.9882(3) 0.1501(3) 0.91093(19) 0.0260(7) Uani 1 1 d . . .
H46 H 0.9554 0.0753 0.8818 0.031 Uiso 1 1 calc R . .
C47 C 0.8010(3) 0.1790(3) 0.76445(18) 0.0195(6) Uani 1 1 d . . .
C48 C 0.7071(3) 0.1738(3) 0.71229(19) 0.0241(7) Uani 1 1 d . . .
H48 H 0.6377 0.1587 0.7325 0.029 Uiso 1 1 calc R . .
C49 C 0.7112(3) 0.1897(3) 0.63244(19) 0.0279(7) Uani 1 1 d . . .
H49 H 0.6456 0.1853 0.5995 0.033 Uiso 1 1 calc R . .
C50 C 0.8112(3) 0.2121(3) 0.60087(19) 0.0288(8) Uani 1 1 d . . .
H50 H 0.8145 0.2223 0.5463 0.035 Uiso 1 1 calc R . .
C51 C 0.9051(3) 0.2191(3) 0.64998(19) 0.0275(7) Uani 1 1 d . . .
H51 H 0.9743 0.2348 0.6293 0.033 Uiso 1 1 calc R . .
C52 C 0.9000(3) 0.2035(3) 0.72994(19) 0.0234(7) Uani 1 1 d . . .
H52 H 0.9669 0.2098 0.7624 0.028 Uiso 1 1 calc R . .
C53 C 0.6800(3) 0.5534(4) 0.1548(2) 0.0383(9) Uani 1 1 d . . .
H53A H 0.6744 0.4814 0.1300 0.046 Uiso 1 1 calc R . .
H53B H 0.7620 0.6169 0.1594 0.046 Uiso 1 1 calc R . .
C54 C 0.5990(4) 0.5841(4) 0.1049(3) 0.0444(10) Uani 1 1 d . . .
H54A H 0.5177 0.5230 0.1035 0.067 Uiso 1 1 calc R . .
H54B H 0.6173 0.5909 0.0508 0.067 Uiso 1 1 calc R . .
H54C H 0.6093 0.6584 0.1279 0.067 Uiso 1 1 calc R . .
C55 C 0.7103(4) 0.4945(4) 0.2799(2) 0.0410(9) Uani 1 1 d . . .
H55A H 0.7952 0.5515 0.2883 0.049 Uiso 1 1 calc R . .
H55B H 0.6982 0.4200 0.2543 0.049 Uiso 1 1 calc R . .
C56 C 0.6655(4) 0.4773(4) 0.3579(3) 0.0531(12) Uani 1 1 d . . .
H56A H 0.6796 0.5520 0.3833 0.080 Uiso 1 1 calc R . .
H56B H 0.7065 0.4468 0.3926 0.080 Uiso 1 1 calc R . .
H56C H 0.5812 0.4219 0.3487 0.080 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'
B B 0.0013 0.0007 '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'
P P 0.1023 0.0942 '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'
O O 0.0106 0.0060 '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
C1 Os N3 91.02(13) . . ?
C1 Os N1 87.33(13) . . ?
N3 Os N1 79.64(10) . . ?
C1 Os N5 169.34(13) . . ?
N3 Os N5 88.68(10) . . ?
N1 Os N5 82.13(11) . . ?
C1 Os C9 88.10(17) . . ?
N3 Os C9 156.30(15) . . ?
N1 Os C9 76.65(15) . . ?
N5 Os C9 87.91(15) . . ?
C1 Os C10 95.18(16) . . ?
N3 Os C10 167.19(13) . . ?
N1 Os C10 111.78(14) . . ?
N5 Os C10 87.28(13) . . ?
C9 Os C10 35.59(16) . . ?
C1 Os P 95.03(11) . . ?
N3 Os P 88.60(7) . . ?
N1 Os P 168.06(8) . . ?
N5 Os P 95.62(8) . . ?
C9 Os P 115.07(13) . . ?
C10 Os P 79.71(11) . . ?
C26 P C23 102.34(16) . . ?
C26 P C20 106.30(16) . . ?
C23 P C20 101.40(17) . . ?
C26 P Os 112.01(12) . . ?
C23 P Os 114.34(11) . . ?
C20 P Os 118.70(13) . . ?
C53 O C55 112.2(3) . . ?
C11 N1 N2 106.6(3) . . ?
C11 N1 Os 132.2(2) . . ?
N2 N1 Os 120.9(2) . . ?
C13 N2 N1 109.4(3) . . ?
C13 N2 B1 130.5(3) . . ?
N1 N2 B1 119.7(3) . . ?
C14 N3 N4 106.4(3) . . ?
C14 N3 Os 132.9(2) . . ?
N4 N3 Os 120.34(19) . . ?
C16 N4 N3 109.2(3) . . ?
C16 N4 B1 128.6(3) . . ?
N3 N4 B1 120.3(3) . . ?
C17 N5 N6 106.1(3) . . ?
C17 N5 Os 135.6(2) . . ?
N6 N5 Os 118.16(19) . . ?
C19 N6 N5 108.7(3) . . ?
C19 N6 B1 129.0(3) . . ?
N5 N6 B1 120.9(3) . . ?
N6 B1 N2 109.4(3) . . ?
N6 B1 N4 110.0(3) . . ?
N2 B1 N4 105.0(3) . . ?
N6 B1 H1 112.7(18) . . ?
N2 B1 H1 110.2(19) . . ?
N4 B1 H1 109.3(19) . . ?
C35 B2 C47 109.2(2) . . ?
C35 B2 C41 111.0(3) . . ?
C47 B2 C41 108.7(3) . . ?
C35 B2 C29 108.8(2) . . ?
C47 B2 C29 111.1(2) . . ?
C41 B2 C29 108.0(2) . . ?
C2 C1 Os 169.2(3) . . ?
C1 C2 C3 127.6(3) . . ?
C1 C2 H2 115(3) . . ?
C3 C2 H2 118(3) . . ?
C8 C3 C4 118.3(4) . . ?
C8 C3 C2 122.9(3) . . ?
C4 C3 C2 118.9(3) . . ?
C5 C4 C3 120.4(4) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C6 C5 C4 121.0(4) . . ?
C6 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
C5 C6 C7 118.6(4) . . ?
C5 C6 H6 120.7 . . ?
C7 C6 H6 120.7 . . ?
C6 C7 C8 120.9(4) . . ?
C6 C7 H7 119.6 . . ?
C8 C7 H7 119.6 . . ?
C7 C8 C3 120.8(4) . . ?
C7 C8 H8 119.6 . . ?
C3 C8 H8 119.6 . . ?
C10 C9 Os 72.9(2) . . ?
C10 C9 H9A 119(3) . . ?
Os C9 H9A 103(2) . . ?
C10 C9 H9B 119(3) . . ?
Os C9 H9B 106(3) . . ?
H9A C9 H9B 120(4) . . ?
C9 C10 Os 71.6(2) . . ?
C9 C10 H10A 121(2) . . ?
Os C10 H10A 109(2) . . ?
C9 C10 H10B 122(3) . . ?
Os C10 H10B 108(2) . . ?
H10A C10 H10B 114(3) . . ?
N1 C11 C12 109.9(3) . . ?
N1 C11 H11 125.1 . . ?
C12 C11 H11 125.1 . . ?
C13 C12 C11 105.2(3) . . ?
C13 C12 H12 127.4 . . ?
C11 C12 H12 127.4 . . ?
N2 C13 C12 108.8(3) . . ?
N2 C13 H13 125.6 . . ?
C12 C13 H13 125.6 . . ?
N3 C14 C15 110.2(3) . . ?
N3 C14 H14 124.9 . . ?
C15 C14 H14 124.9 . . ?
C16 C15 C14 105.1(3) . . ?
C16 C15 H15 127.4 . . ?
C14 C15 H15 127.4 . . ?
N4 C16 C15 109.1(3) . . ?
N4 C16 H16 125.4 . . ?
C15 C16 H16 125.4 . . ?
N5 C17 C18 110.9(3) . . ?
N5 C17 H17 124.6 . . ?
C18 C17 H17 124.6 . . ?
C19 C18 C17 105.0(3) . . ?
C19 C18 H18 127.5 . . ?
C17 C18 H18 127.5 . . ?
N6 C19 C18 109.3(3) . . ?
N6 C19 H19 125.3 . . ?
C18 C19 H19 125.3 . . ?
C22 C20 C21 108.9(3) . . ?
C22 C20 P 116.0(3) . . ?
C21 C20 P 112.7(3) . . ?
C22 C20 H20 106.2 . . ?
C21 C20 H20 106.2 . . ?
P C20 H20 106.2 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 C25 110.8(3) . . ?
C24 C23 P 112.4(2) . . ?
C25 C23 P 115.0(3) . . ?
C24 C23 H23 106.0 . . ?
C25 C23 H23 106.0 . . ?
P C23 H23 106.0 . . ?
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 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C28 C26 C27 109.7(3) . . ?
C28 C26 P 115.8(3) . . ?
C27 C26 P 115.2(2) . . ?
C28 C26 H26 104.9 . . ?
C27 C26 H26 104.9 . . ?
P C26 H26 104.9 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 C34 115.0(3) . . ?
C30 C29 B2 122.8(3) . . ?
C34 C29 B2 122.1(3) . . ?
C31 C30 C29 122.8(3) . . ?
C31 C30 H30 118.6 . . ?
C29 C30 H30 118.6 . . ?
C32 C31 C30 120.0(3) . . ?
C32 C31 H31 120.0 . . ?
C30 C31 H31 120.0 . . ?
C31 C32 C33 118.9(3) . . ?
C31 C32 H32 120.5 . . ?
C33 C32 H32 120.5 . . ?
C34 C33 C32 120.2(3) . . ?
C34 C33 H33 119.9 . . ?
C32 C33 H33 119.9 . . ?
C33 C34 C29 123.0(3) . . ?
C33 C34 H34 118.5 . . ?
C29 C34 H34 118.5 . . ?
C36 C35 C40 114.7(3) . . ?
C36 C35 B2 122.8(3) . . ?
C40 C35 B2 122.3(3) . . ?
C37 C36 C35 122.9(3) . . ?
C37 C36 H36 118.5 . . ?
C35 C36 H36 118.5 . . ?
C38 C37 C36 120.3(3) . . ?
C38 C37 H37 119.8 . . ?
C36 C37 H37 119.8 . . ?
C37 C38 C39 119.1(3) . . ?
C37 C38 H38 120.4 . . ?
C39 C38 H38 120.4 . . ?
C38 C39 C40 120.1(3) . . ?
C38 C39 H39 120.0 . . ?
C40 C39 H39 120.0 . . ?
C39 C40 C35 122.9(3) . . ?
C39 C40 H40 118.6 . . ?
C35 C40 H40 118.6 . . ?
C42 C41 C46 114.8(3) . . ?
C42 C41 B2 123.4(3) . . ?
C46 C41 B2 121.8(3) . . ?
C43 C42 C41 123.1(3) . . ?
C43 C42 H42 118.4 . . ?
C41 C42 H42 118.4 . . ?
C44 C43 C42 120.3(3) . . ?
C44 C43 H43 119.9 . . ?
C42 C43 H43 119.9 . . ?
C43 C44 C45 119.0(3) . . ?
C43 C44 H44 120.5 . . ?
C45 C44 H44 120.5 . . ?
C44 C45 C46 120.1(3) . . ?
C44 C45 H45 119.9 . . ?
C46 C45 H45 119.9 . . ?
C45 C46 C41 122.7(3) . . ?
C45 C46 H46 118.6 . . ?
C41 C46 H46 118.6 . . ?
C52 C47 C48 114.5(3) . . ?
C52 C47 B2 123.7(3) . . ?
C48 C47 B2 121.6(3) . . ?
C49 C48 C47 123.0(3) . . ?
C49 C48 H48 118.5 . . ?
C47 C48 H48 118.5 . . ?
C50 C49 C48 120.1(3) . . ?
C50 C49 H49 120.0 . . ?
C48 C49 H49 120.0 . . ?
C51 C50 C49 118.7(3) . . ?
C51 C50 H50 120.7 . . ?
C49 C50 H50 120.7 . . ?
C50 C51 C52 120.6(3) . . ?
C50 C51 H51 119.7 . . ?
C52 C51 H51 119.7 . . ?
C51 C52 C47 123.0(3) . . ?
C51 C52 H52 118.5 . . ?
C47 C52 H52 118.5 . . ?
O C53 C54 108.2(3) . . ?
O C53 H53A 110.1 . . ?
C54 C53 H53A 110.1 . . ?
O C53 H53B 110.1 . . ?
C54 C53 H53B 110.1 . . ?
H53A C53 H53B 108.4 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
O C55 C56 107.5(3) . . ?
O C55 H55A 110.2 . . ?
C56 C55 H55A 110.2 . . ?
O C55 H55B 110.2 . . ?
C56 C55 H55B 110.2 . . ?
H55A C55 H55B 108.5 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 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
Os C1 1.841(3) . ?
Os N3 2.124(3) . ?
Os N1 2.149(3) . ?
Os N5 2.199(3) . ?
Os C9 2.216(4) . ?
Os C10 2.232(4) . ?
Os P 2.4570(9) . ?
P C26 1.856(3) . ?
P C23 1.860(3) . ?
P C20 1.869(3) . ?
O C53 1.411(4) . ?
O C55 1.430(4) . ?
N1 C11 1.342(4) . ?
N1 N2 1.358(4) . ?
N2 C13 1.340(4) . ?
N2 B1 1.537(4) . ?
N3 C14 1.343(4) . ?
N3 N4 1.363(4) . ?
N4 C16 1.340(4) . ?
N4 B1 1.544(5) . ?
N5 C17 1.343(4) . ?
N5 N6 1.376(4) . ?
N6 C19 1.344(4) . ?
N6 B1 1.511(5) . ?
B1 H1 1.08(4) . ?
B2 C35 1.641(5) . ?
B2 C47 1.647(5) . ?
B2 C41 1.650(5) . ?
B2 C29 1.651(5) . ?
C1 C2 1.312(5) . ?
C2 C3 1.466(5) . ?
C2 H2 0.90(4) . ?
C3 C8 1.385(5) . ?
C3 C4 1.398(5) . ?
C4 C5 1.384(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.381(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.382(6) . ?
C6 H6 0.9500 . ?
C7 C8 1.384(6) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C10 1.360(6) . ?
C9 H9A 0.96(4) . ?
C9 H9B 0.89(4) . ?
C10 H10A 0.96(4) . ?
C10 H10B 0.99(4) . ?
C11 C12 1.386(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.367(5) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C15 1.382(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.366(5) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C18 1.375(5) . ?
C17 H17 0.9500 . ?
C18 C19 1.371(5) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C22 1.530(6) . ?
C20 C21 1.533(5) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.525(5) . ?
C23 C25 1.529(5) . ?
C23 H23 1.0000 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C28 1.538(5) . ?
C26 C27 1.540(5) . ?
C26 H26 1.0000 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.399(4) . ?
C29 C34 1.408(4) . ?
C30 C31 1.396(4) . ?
C30 H30 0.9500 . ?
C31 C32 1.385(5) . ?
C31 H31 0.9500 . ?
C32 C33 1.387(5) . ?
C32 H32 0.9500 . ?
C33 C34 1.381(4) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C35 C36 1.403(4) . ?
C35 C40 1.403(4) . ?
C36 C37 1.386(5) . ?
C36 H36 0.9500 . ?
C37 C38 1.376(5) . ?
C37 H37 0.9500 . ?
C38 C39 1.378(5) . ?
C38 H38 0.9500 . ?
C39 C40 1.390(5) . ?
C39 H39 0.9500 . ?
C40 H40 0.9500 . ?
C41 C42 1.391(4) . ?
C41 C46 1.404(4) . ?
C42 C43 1.387(4) . ?
C42 H42 0.9500 . ?
C43 C44 1.374(5) . ?
C43 H43 0.9500 . ?
C44 C45 1.377(5) . ?
C44 H44 0.9500 . ?
C45 C46 1.389(5) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C47 C52 1.397(4) . ?
C47 C48 1.407(4) . ?
C48 C49 1.392(4) . ?
C48 H48 0.9500 . ?
C49 C50 1.388(5) . ?
C49 H49 0.9500 . ?
C50 C51 1.371(5) . ?
C50 H50 0.9500 . ?
C51 C52 1.394(4) . ?
C51 H51 0.9500 . ?
C52 H52 0.9500 . ?
C53 C54 1.504(5) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 C56 1.503(6) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
