#------------------------------------------------------------------------------
#$Date: 2018-09-25 10:35:30 +0300 (Tue, 25 Sep 2018) $
#$Revision: 211152 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/30/10/4301026.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_4301026
loop_
_publ_author_name
'Parna Gupta'
'Anindya Das'
'Falguni Basuli'
'Alfonso Castineiras'
'William S. Sheldrick'
'Heike Mayer-Figge'
'Samaresh Bhattacharya'
_publ_section_title
;
 Variable Coordination Mode of Chloranilic Acid. Synthesis, Structure, and
 Electrochemical Properties of Some Osmium Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2081
_journal_page_last               2088
_journal_paper_doi               10.1021/ic049149s
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C53 H41 Cl2 N3 O5 Os P2'
_chemical_formula_weight         1122.93
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 127.15(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.6020(17)
_cell_length_b                   13.2730(15)
_cell_length_c                   25.176(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    208(2)
_cell_measurement_theta_max      13.53
_cell_measurement_theta_min      7.67
_cell_volume                     4688(6)
_computing_cell_refinement       'CAD4-Express Software (Nonius, 1994)'
_computing_data_collection       'CAD4-Express Software (Nonius, 1994)'
_computing_data_reduction        'GENHKL (kretschmar, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      208(2)
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'CAD4 Enraf Nonius'
_diffrn_measurement_method       omega
_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  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0711
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            10930
_diffrn_reflns_theta_full        25.96
_diffrn_reflns_theta_max         25.96
_diffrn_reflns_theta_min         3.06
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.955
_exptl_absorpt_correction_T_max  0.8663
_exptl_absorpt_correction_T_min  0.4710
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.970
_refine_diff_density_min         -1.325
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         9109
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0383P)²+4.1601P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0916
_reflns_number_gt                6376
_reflns_number_total             9109
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049149ssi20040629_024951.cif
_cod_data_source_block           acs3
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2018-09-25

The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'Psi-scans' was replaced
with 'psi-scan' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0383P)^2^+4.1601P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0383P)^2^+4.1601P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4688.3(9)
_cod_database_code               4301026
loop_
_symmetry_equiv_pos_as_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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Os1 Os 0.268193(15) 0.239323(15) 0.010333(11) 0.03219(7) Uani 1 d . . . 0
Cl1 Cl 0.04713(11) 0.24199(12) -0.24116(7) 0.0551(4) Uani 1 d . . . 0
Cl2 Cl 0.36201(13) -0.08127(13) -0.04866(9) 0.0644(5) Uani 1 d . . . 0
P1 P 0.36371(10) 0.35312(11) -0.00250(8) 0.0344(3) Uani 1 d . . . 0
P2 P 0.16587(10) 0.12248(11) 0.01300(7) 0.0332(3) Uani 1 d . . . 0
O1 O 0.1794(2) 0.2398(3) -0.09338(18) 0.0367(8) Uani 1 d . . . 0
O2 O 0.3143(2) 0.1122(3) -0.01405(18) 0.0339(8) Uani 1 d . . . 0
O3 O 0.2196(4) -0.0919(4) -0.1970(3) 0.095(2) Uani 1 d . . . 0
O4 O 0.0863(4) 0.0454(4) -0.2794(2) 0.0669(14) Uani 1 d . . . 0
N11 N 0.2096(4) 0.3545(4) 0.0251(3) 0.0502(14) Uani 1 d . . . 0
N12 N 0.3281(5) 0.3197(5) 0.1367(3) 0.0717(19) Uani 1 d . . . 0
N13 N 0.3469(3) 0.2499(4) 0.1072(2) 0.0489(13) Uani 1 d . . . 0
C1 C 0.1309(4) 0.1510(4) -0.1901(3) 0.0404(13) Uani 1 d . . . 0
C2 C 0.1855(4) 0.1632(4) -0.1228(3) 0.0314(12) Uani 1 d . . . 0
C3 C 0.2620(4) 0.0890(4) -0.0764(3) 0.0354(13) Uani 1 d . . . 0
C4 C 0.2721(4) 0.0030(4) -0.1024(3) 0.0417(14) Uani 1 d . . . 0
C5 C 0.2145(5) -0.0164(5) -0.1714(3) 0.0513(16) Uani 1 d . . . 0
C6 C 0.1365(4) 0.0622(5) -0.2197(3) 0.0482(15) Uani 1 d . . . 0
C11 C 0.1328(5) 0.4081(5) -0.0207(4) 0.061(2) Uani 1 d . . . 0
H11 H 0.1024 0.3929 -0.0658 0.074 Uiso 1 calc R . . 0
C12 C 0.0956(6) 0.4838(6) -0.0060(6) 0.092(3) Uani 1 d . . . 0
H12 H 0.0416 0.5197 -0.0402 0.110 Uiso 1 calc R . . 0
C13 C 0.1382(8) 0.5063(7) 0.0591(7) 0.109(4) Uani 1 d . . . 0
H13 H 0.1141 0.5589 0.0700 0.130 Uiso 1 calc R . . 0
C14 C 0.2151(7) 0.4531(7) 0.1083(5) 0.094(3) Uani 1 d . . . 0
H14 H 0.2441 0.4671 0.1534 0.113 Uiso 1 calc R . . 0
C15 C 0.2510(6) 0.3749(6) 0.0894(5) 0.071(2) Uani 1 d . . . 0
C16 C 0.4274(5) 0.1886(6) 0.1538(3) 0.0606(19) Uani 1 d . . . 0
C17 C 0.4513(7) 0.1726(9) 0.2167(4) 0.107(4) Uani 1 d . . . 0
H17 H 0.4151 0.2014 0.2289 0.128 Uiso 1 calc R . . 0
C18 C 0.5288(12) 0.1142(14) 0.2603(8) 0.170(8) Uani 1 d . . . 0
H18 H 0.5464 0.1030 0.3032 0.204 Uiso 1 calc R . . 0
C19 C 0.5800(12) 0.0727(15) 0.2433(8) 0.193(10) Uani 1 d . . . 0
H19 H 0.6315 0.0307 0.2740 0.232 Uiso 1 calc R . . 0
C20 C 0.5595(7) 0.0897(8) 0.1804(6) 0.118(4) Uani 1 d . . . 0
H20 H 0.5978 0.0628 0.1693 0.141 Uiso 1 calc R . . 0
C21 C 0.4798(4) 0.1481(5) 0.1357(4) 0.064(2) Uani 1 d . . . 0
H21 H 0.4619 0.1598 0.0927 0.077 Uiso 1 calc R . . 0
C31 C 0.3084(4) 0.4781(4) -0.0312(3) 0.0392(13) Uani 1 d . . . 0
C32 C 0.2163(4) 0.4830(5) -0.0902(3) 0.0468(15) Uani 1 d . . . 0
H32 H 0.1860 0.4238 -0.1146 0.056 Uiso 1 calc R . . 0
C33 C 0.1686(5) 0.5743(5) -0.1134(4) 0.0577(18) Uani 1 d . . . 0
H33 H 0.1071 0.5775 -0.1541 0.069 Uiso 1 calc R . . 0
C34 C 0.2122(6) 0.6602(5) -0.0762(4) 0.064(2) Uani 1 d . . . 0
H34 H 0.1793 0.7219 -0.0909 0.077 Uiso 1 calc R . . 0
C35 C 0.3041(5) 0.6565(5) -0.0171(4) 0.0615(19) Uani 1 d . . . 0
H35 H 0.3337 0.7154 0.0080 0.074 Uiso 1 calc R . . 0
C36 C 0.3515(4) 0.5655(4) 0.0044(3) 0.0453(15) Uani 1 d . . . 0
H36 H 0.4142 0.5630 0.0440 0.054 Uiso 1 calc R . . 0
C41 C 0.3829(4) 0.3111(4) -0.0627(3) 0.0381(13) Uani 1 d . . . 0
C42 C 0.4233(4) 0.2162(4) -0.0544(3) 0.0438(15) Uani 1 d . . . 0
H42 H 0.4435 0.1773 -0.0168 0.053 Uiso 1 calc R . . 0
C43 C 0.4339(5) 0.1792(5) -0.1005(3) 0.0533(17) Uani 1 d . . . 0
H43 H 0.4612 0.1154 -0.0942 0.064 Uiso 1 calc R . . 0
C44 C 0.4045(5) 0.2356(5) -0.1559(3) 0.0615(18) Uani 1 d . . . 0
H44 H 0.4099 0.2099 -0.1882 0.074 Uiso 1 calc R . . 0
C45 C 0.3668(5) 0.3304(5) -0.1630(3) 0.0613(19) Uani 1 d . . . 0
H45 H 0.3487 0.3698 -0.2000 0.074 Uiso 1 calc R . . 0
C46 C 0.3553(4) 0.3684(5) -0.1180(3) 0.0494(16) Uani 1 d . . . 0
H46 H 0.3289 0.4329 -0.1242 0.059 Uiso 1 calc R . . 0
C51 C 0.4831(4) 0.3734(4) 0.0754(3) 0.0385(13) Uani 1 d . . . 0
C52 C 0.4911(4) 0.4121(4) 0.1299(3) 0.0424(14) Uani 1 d . . . 0
H52 H 0.4362 0.4347 0.1246 0.051 Uiso 1 calc R . . 0
C53 C 0.5782(5) 0.4177(5) 0.1916(3) 0.0571(18) Uani 1 d . . . 0
H53 H 0.5827 0.4446 0.2279 0.069 Uiso 1 calc R . . 0
C54 C 0.6591(5) 0.3839(6) 0.2001(4) 0.064(2) Uani 1 d . . . 0
H54 H 0.7186 0.3865 0.2424 0.077 Uiso 1 calc R . . 0
C55 C 0.6519(5) 0.3459(6) 0.1458(4) 0.0627(19) Uani 1 d . . . 0
H55 H 0.7068 0.3229 0.1514 0.075 Uiso 1 calc R . . 0
C56 C 0.5644(4) 0.3417(5) 0.0836(3) 0.0465(15) Uani 1 d . . . 0
H56 H 0.5602 0.3174 0.0468 0.056 Uiso 1 calc R . . 0
C61 C 0.0693(4) 0.0782(4) -0.0705(3) 0.0350(12) Uani 1 d . . . 0
C62 C 0.0069(4) 0.1481(5) -0.1197(3) 0.0404(14) Uani 1 d . . . 0
H62 H 0.0116 0.2168 -0.1089 0.049 Uiso 1 calc R . . 0
C63 C -0.0613(4) 0.1163(6) -0.1838(3) 0.0565(18) Uani 1 d . . . 0
H63 H -0.1043 0.1630 -0.2166 0.068 Uiso 1 calc R . . 0
C64 C -0.0671(5) 0.0154(6) -0.2003(4) 0.068(2) Uani 1 d . . . 0
H64 H -0.1140 -0.0064 -0.2442 0.082 Uiso 1 calc R . . 0
C65 C -0.0047(6) -0.0517(6) -0.1529(4) 0.072(2) Uani 1 d . . . 0
H65 H -0.0073 -0.1196 -0.1645 0.086 Uiso 1 calc R . . 0
C66 C 0.0626(5) -0.0215(4) -0.0878(3) 0.0473(15) Uani 1 d . . . 0
H66 H 0.1040 -0.0692 -0.0552 0.057 Uiso 1 calc R . . 0
C71 C 0.1119(4) 0.1785(4) 0.0491(3) 0.0386(13) Uani 1 d . . . 0
C72 C 0.1686(4) 0.1895(5) 0.1184(3) 0.0533(17) Uani 1 d . . . 0
H72 H 0.2302 0.1617 0.1453 0.064 Uiso 1 calc R . . 0
C73 C 0.1339(5) 0.2411(6) 0.1470(4) 0.066(2) Uani 1 d . . . 0
H73 H 0.1730 0.2497 0.1935 0.080 Uiso 1 calc R . . 0
C74 C 0.0438(6) 0.2803(5) 0.1093(4) 0.069(2) Uani 1 d . . . 0
H74 H 0.0214 0.3162 0.1296 0.082 Uiso 1 calc R . . 0
C75 C -0.0129(5) 0.2667(5) 0.0423(4) 0.0580(17) Uani 1 d . . . 0
H75 H -0.0757 0.2913 0.0161 0.070 Uiso 1 calc R . . 0
C76 C 0.0208(4) 0.2168(4) 0.0120(3) 0.0464(15) Uani 1 d . . . 0
H76 H -0.0191 0.2090 -0.0346 0.056 Uiso 1 calc R . . 0
C81 C 0.2193(4) 0.0078(4) 0.0618(3) 0.0397(14) Uani 1 d . . . 0
C82 C 0.1737(4) -0.0448(5) 0.0840(3) 0.0494(16) Uani 1 d . . . 0
H82 H 0.1173 -0.0194 0.0753 0.059 Uiso 1 calc R . . 0
C83 C 0.2127(5) -0.1344(5) 0.1189(3) 0.0585(18) Uani 1 d . . . 0
H83 H 0.1815 -0.1701 0.1329 0.070 Uiso 1 calc R . . 0
C84 C 0.2959(5) -0.1717(5) 0.1332(3) 0.064(2) Uani 1 d . . . 0
H84 H 0.3222 -0.2316 0.1577 0.077 Uiso 1 calc R . . 0
C85 C 0.3406(5) -0.1207(5) 0.1112(4) 0.0617(19) Uani 1 d . . . 0
H85 H 0.3971 -0.1466 0.1204 0.074 Uiso 1 calc R . . 0
C86 C 0.3024(4) -0.0311(5) 0.0756(3) 0.0475(15) Uani 1 d . . . 0
H86 H 0.3333 0.0030 0.0608 0.057 Uiso 1 calc R . . 0
O10 O 0.1189(7) -0.1296(5) -0.3339(3) 0.147(3) Uani 1 d . . . 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Os Os -1.2165 7.6030 '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'
P P 0.1023 0.0942 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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
N13 Os1 N11 76.7(2) . . y
N13 Os1 O1 175.19(19) . . y
N11 Os1 O1 98.6(2) . . y
N13 Os1 O2 108.2(2) . . y
N11 Os1 O2 173.51(18) . . y
O1 Os1 O2 76.57(14) . . y
N13 Os1 P2 89.42(15) . . y
N11 Os1 P2 90.50(14) . . y
O1 Os1 P2 91.70(12) . . y
O2 Os1 P2 85.36(10) . . y
N13 Os1 P1 95.49(15) . . y
N11 Os1 P1 91.47(14) . . y
O1 Os1 P1 83.47(12) . . y
O2 Os1 P1 92.28(10) . . y
P2 Os1 P1 175.01(5) . . y
C41 P1 C51 105.5(3) . . ?
C41 P1 C31 105.6(3) . . ?
C51 P1 C31 106.3(3) . . ?
C41 P1 Os1 114.24(19) . . ?
C51 P1 Os1 112.85(19) . . ?
C31 P1 Os1 111.72(18) . . ?
C81 P2 C71 102.5(3) . . ?
C81 P2 C61 104.5(3) . . ?
C71 P2 C61 107.6(3) . . ?
C81 P2 Os1 117.8(2) . . ?
C71 P2 Os1 112.03(18) . . ?
C61 P2 Os1 111.50(18) . . ?
C2 O1 Os1 117.1(3) . . ?
C3 O2 Os1 115.2(3) . . ?
C5 O3 O10 126.8(5) . . ?
C6 O4 O10 121.5(5) . . ?
C11 N11 C15 117.6(7) . . ?
C11 N11 Os1 127.9(5) . . ?
C15 N11 Os1 114.4(5) . . ?
N13 N12 C15 109.6(6) . . ?
N12 N13 C16 113.0(6) . . ?
N12 N13 Os1 120.8(5) . . ?
C16 N13 Os1 126.2(5) . . ?
C2 C1 C6 121.9(5) . . ?
C2 C1 Cl1 119.1(5) . . ?
C6 C1 Cl1 118.9(5) . . ?
O1 C2 C1 124.3(5) . . ?
O1 C2 C3 114.4(5) . . ?
C1 C2 C3 121.3(5) . . ?
O2 C3 C4 125.0(5) . . ?
O2 C3 C2 115.9(5) . . ?
C4 C3 C2 119.0(5) . . ?
C3 C4 C5 122.3(5) . . ?
C3 C4 Cl2 118.8(5) . . ?
C5 C4 Cl2 118.9(4) . . ?
O3 C5 C4 124.9(6) . . ?
O3 C5 C6 116.5(6) . . ?
C4 C5 C6 118.6(5) . . ?
O4 C6 C1 124.6(6) . . ?
O4 C6 C5 118.7(6) . . ?
C1 C6 C5 116.7(5) . . ?
N11 C11 C12 124.0(8) . . ?
N11 C11 H11 118.0 . . ?
C12 C11 H11 118.0 . . ?
C13 C12 C11 118.8(9) . . ?
C13 C12 H12 120.6 . . ?
C11 C12 H12 120.6 . . ?
C12 C13 C14 120.4(8) . . ?
C12 C13 H13 119.8 . . ?
C14 C13 H13 119.8 . . ?
C13 C14 C15 118.0(9) . . ?
C13 C14 H14 121.0 . . ?
C15 C14 H14 121.0 . . ?
N11 C15 N12 118.5(7) . . ?
N11 C15 C14 121.2(9) . . ?
N12 C15 C14 120.4(9) . . ?
C21 C16 C17 121.5(9) . . ?
C21 C16 N13 119.0(6) . . ?
C17 C16 N13 119.5(8) . . ?
C18 C17 C16 118.1(12) . . ?
C18 C17 H17 120.9 . . ?
C16 C17 H17 120.9 . . ?
C19 C18 C17 121.4(16) . . ?
C19 C18 H18 119.3 . . ?
C17 C18 H18 119.3 . . ?
C18 C19 C20 122.1(15) . . ?
C18 C19 H19 119.0 . . ?
C20 C19 H19 119.0 . . ?
C21 C20 C19 116.5(12) . . ?
C21 C20 H20 121.8 . . ?
C19 C20 H20 121.8 . . ?
C16 C21 C20 120.4(9) . . ?
C16 C21 H21 119.8 . . ?
C20 C21 H21 119.8 . . ?
C36 C31 C32 118.9(5) . . ?
C36 C31 P1 123.4(5) . . ?
C32 C31 P1 117.6(4) . . ?
C31 C32 C33 120.7(6) . . ?
C31 C32 H32 119.6 . . ?
C33 C32 H32 119.6 . . ?
C34 C33 C32 119.3(6) . . ?
C34 C33 H33 120.3 . . ?
C32 C33 H33 120.3 . . ?
C33 C34 C35 120.6(6) . . ?
C33 C34 H34 119.7 . . ?
C35 C34 H34 119.7 . . ?
C36 C35 C34 119.3(6) . . ?
C36 C35 H35 120.3 . . ?
C34 C35 H35 120.3 . . ?
C35 C36 C31 121.1(6) . . ?
C35 C36 H36 119.5 . . ?
C31 C36 H36 119.5 . . ?
C46 C41 C42 118.7(6) . . ?
C46 C41 P1 122.3(5) . . ?
C42 C41 P1 118.9(4) . . ?
C43 C42 C41 120.8(6) . . ?
C43 C42 H42 119.6 . . ?
C41 C42 H42 119.6 . . ?
C42 C43 C44 120.1(6) . . ?
C42 C43 H43 120.0 . . ?
C44 C43 H43 120.0 . . ?
C43 C44 C45 118.9(6) . . ?
C43 C44 H44 120.6 . . ?
C45 C44 H44 120.6 . . ?
C46 C45 C44 122.0(7) . . ?
C46 C45 H45 119.0 . . ?
C44 C45 H45 119.0 . . ?
C45 C46 C41 119.4(6) . . ?
C45 C46 H46 120.3 . . ?
C41 C46 H46 120.3 . . ?
C56 C51 C52 119.1(5) . . ?
C56 C51 P1 121.9(5) . . ?
C52 C51 P1 118.6(4) . . ?
C53 C52 C51 120.8(6) . . ?
C53 C52 H52 119.6 . . ?
C51 C52 H52 119.6 . . ?
C52 C53 C54 120.1(7) . . ?
C52 C53 H53 120.0 . . ?
C54 C53 H53 120.0 . . ?
C53 C54 C55 119.5(6) . . ?
C53 C54 H54 120.3 . . ?
C55 C54 H54 120.3 . . ?
C56 C55 C54 120.4(6) . . ?
C56 C55 H55 119.8 . . ?
C54 C55 H55 119.8 . . ?
C55 C56 C51 120.0(6) . . ?
C55 C56 H56 120.0 . . ?
C51 C56 H56 120.0 . . ?
C66 C61 C62 119.1(5) . . ?
C66 C61 P2 121.1(5) . . ?
C62 C61 P2 119.6(4) . . ?
C63 C62 C61 119.9(6) . . ?
C63 C62 H62 120.0 . . ?
C61 C62 H62 120.0 . . ?
C62 C63 C64 120.2(7) . . ?
C62 C63 H63 119.9 . . ?
C64 C63 H63 119.9 . . ?
C65 C64 C63 119.7(7) . . ?
C65 C64 H64 120.2 . . ?
C63 C64 H64 120.2 . . ?
C64 C65 C66 120.9(7) . . ?
C64 C65 H65 119.6 . . ?
C66 C65 H65 119.6 . . ?
C65 C66 C61 120.2(6) . . ?
C65 C66 H66 119.9 . . ?
C61 C66 H66 119.9 . . ?
C76 C71 C72 118.1(6) . . ?
C76 C71 P2 123.7(5) . . ?
C72 C71 P2 118.0(5) . . ?
C73 C72 C71 119.8(6) . . ?
C73 C72 H72 120.1 . . ?
C71 C72 H72 120.1 . . ?
C74 C73 C72 121.5(7) . . ?
C74 C73 H73 119.3 . . ?
C72 C73 H73 119.3 . . ?
C73 C74 C75 119.1(7) . . ?
C73 C74 H74 120.5 . . ?
C75 C74 H74 120.5 . . ?
C74 C75 C76 120.7(7) . . ?
C74 C75 H75 119.6 . . ?
C76 C75 H75 119.6 . . ?
C71 C76 C75 120.8(6) . . ?
C71 C76 H76 119.6 . . ?
C75 C76 H76 119.6 . . ?
C86 C81 C82 119.0(6) . . ?
C86 C81 P2 121.2(5) . . ?
C82 C81 P2 119.7(4) . . ?
C83 C82 C81 119.5(6) . . ?
C83 C82 H82 120.3 . . ?
C81 C82 H82 120.3 . . ?
C84 C83 C82 121.1(6) . . ?
C84 C83 H83 119.4 . . ?
C82 C83 H83 119.4 . . ?
C83 C84 C85 119.6(6) . . ?
C83 C84 H84 120.2 . . ?
C85 C84 H84 120.2 . . ?
C84 C85 C86 120.4(6) . . ?
C84 C85 H85 119.8 . . ?
C86 C85 H85 119.8 . . ?
C81 C86 C85 120.3(6) . . ?
C81 C86 H86 119.8 . . ?
C85 C86 H86 119.8 . . ?
O3 O10 O4 55.98(18) . . ?
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 N13 1.951(5) . y
Os1 N11 2.001(5) . y
Os1 O1 2.081(5) . y
Os1 O2 2.117(4) . y
Os1 P2 2.4083(14) . y
Os1 P1 2.4224(15) . y
Cl1 C1 1.731(6) . ?
Cl2 C4 1.732(6) . ?
P1 C41 1.828(6) . ?
P1 C51 1.833(6) . ?
P1 C31 1.836(6) . ?
P2 C81 1.821(6) . ?
P2 C71 1.825(6) . ?
P2 C61 1.827(6) . ?
O1 C2 1.300(6) . ?
O2 C3 1.288(7) . ?
O3 C5 1.224(7) . ?
O3 O10 2.809(8) . ?
O4 C6 1.218(7) . ?
O4 O10 2.924(9) . ?
N11 C11 1.334(9) . ?
N11 C15 1.342(9) . ?
N12 N13 1.349(7) . ?
N12 C15 1.358(10) . ?
N13 C16 1.428(9) . ?
C1 C2 1.361(8) . ?
C1 C6 1.430(8) . ?
C2 C3 1.500(7) . ?
C3 C4 1.380(8) . ?
C4 C5 1.408(8) . ?
C5 C6 1.561(9) . ?
C11 C12 1.366(9) . ?
C11 H11 0.9400 . ?
C12 C13 1.361(13) . ?
C12 H12 0.9400 . ?
C13 C14 1.356(14) . ?
C13 H13 0.9400 . ?
C14 C15 1.437(10) . ?
C14 H14 0.9400 . ?
C16 C21 1.362(10) . ?
C16 C17 1.387(10) . ?
C17 C18 1.363(17) . ?
C17 H17 0.9400 . ?
C18 C19 1.33(2) . ?
C18 H18 0.9400 . ?
C19 C20 1.414(19) . ?
C19 H19 0.9400 . ?
C20 C21 1.389(11) . ?
C20 H20 0.9400 . ?
C21 H21 0.9400 . ?
C31 C36 1.381(8) . ?
C31 C32 1.389(8) . ?
C32 C33 1.386(8) . ?
C32 H32 0.9400 . ?
C33 C34 1.378(10) . ?
C33 H33 0.9400 . ?
C34 C35 1.388(10) . ?
C34 H34 0.9400 . ?
C35 C36 1.379(8) . ?
C35 H35 0.9400 . ?
C36 H36 0.9400 . ?
C41 C46 1.391(8) . ?
C41 C42 1.398(8) . ?
C42 C43 1.372(8) . ?
C42 H42 0.9400 . ?
C43 C44 1.378(9) . ?
C43 H43 0.9400 . ?
C44 C45 1.383(9) . ?
C44 H44 0.9400 . ?
C45 C46 1.363(9) . ?
C45 H45 0.9400 . ?
C46 H46 0.9400 . ?
C51 C56 1.383(8) . ?
C51 C52 1.390(8) . ?
C52 C53 1.375(8) . ?
C52 H52 0.9400 . ?
C53 C54 1.380(9) . ?
C53 H53 0.9400 . ?
C54 C55 1.389(10) . ?
C54 H54 0.9400 . ?
C55 C56 1.385(9) . ?
C55 H55 0.9400 . ?
C56 H56 0.9400 . ?
C61 C66 1.376(8) . ?
C61 C62 1.400(8) . ?
C62 C63 1.372(8) . ?
C62 H62 0.9400 . ?
C63 C64 1.389(10) . ?
C63 H63 0.9400 . ?
C64 C65 1.357(10) . ?
C64 H64 0.9400 . ?
C65 C66 1.380(9) . ?
C65 H65 0.9400 . ?
C66 H66 0.9400 . ?
C71 C76 1.375(8) . ?
C71 C72 1.398(8) . ?
C72 C73 1.375(9) . ?
C72 H72 0.9400 . ?
C73 C74 1.366(10) . ?
C73 H73 0.9400 . ?
C74 C75 1.358(10) . ?
C74 H74 0.9400 . ?
C75 C76 1.385(8) . ?
C75 H75 0.9400 . ?
C76 H76 0.9400 . ?
C81 C86 1.384(8) . ?
C81 C82 1.410(8) . ?
C82 C83 1.389(9) . ?
C82 H82 0.9400 . ?
C83 C84 1.372(9) . ?
C83 H83 0.9400 . ?
C84 C85 1.382(9) . ?
C84 H84 0.9400 . ?
C85 C86 1.394(8) . ?
C85 H85 0.9400 . ?
C86 H86 0.9400 . ?
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
N13 Os1 P1 C41 137.7(3) . . . . ?
N11 Os1 P1 C41 -145.5(3) . . . . ?
O1 Os1 P1 C41 -47.0(2) . . . . ?
O2 Os1 P1 C41 29.2(2) . . . . ?
P2 Os1 P1 C41 -32.3(6) . . . . ?
N13 Os1 P1 C51 17.3(3) . . . . ?
N11 Os1 P1 C51 94.1(3) . . . . ?
O1 Os1 P1 C51 -167.4(2) . . . . ?
O2 Os1 P1 C51 -91.2(2) . . . . ?
P2 Os1 P1 C51 -152.8(6) . . . . ?
N13 Os1 P1 C31 -102.5(3) . . . . ?
N11 Os1 P1 C31 -25.7(3) . . . . ?
O1 Os1 P1 C31 72.8(2) . . . . ?
O2 Os1 P1 C31 149.0(2) . . . . ?
P2 Os1 P1 C31 87.4(6) . . . . ?
N13 Os1 P2 C81 -58.2(3) . . . . ?
N11 Os1 P2 C81 -134.8(3) . . . . ?
O1 Os1 P2 C81 126.5(2) . . . . ?
O2 Os1 P2 C81 50.1(2) . . . . ?
P1 Os1 P2 C81 112.0(6) . . . . ?
N13 Os1 P2 C71 60.4(3) . . . . ?
N11 Os1 P2 C71 -16.3(3) . . . . ?
O1 Os1 P2 C71 -114.9(2) . . . . ?
O2 Os1 P2 C71 168.7(2) . . . . ?
P1 Os1 P2 C71 -129.5(6) . . . . ?
N13 Os1 P2 C61 -179.0(3) . . . . ?
N11 Os1 P2 C61 104.3(3) . . . . ?
O1 Os1 P2 C61 5.7(2) . . . . ?
O2 Os1 P2 C61 -70.7(2) . . . . ?
P1 Os1 P2 C61 -8.8(6) . . . . ?
N13 Os1 O1 C2 178(22) . . . . ?
N11 Os1 O1 C2 -169.0(3) . . . . ?
O2 Os1 O1 C2 6.5(3) . . . . ?
P2 Os1 O1 C2 -78.3(3) . . . . ?
P1 Os1 O1 C2 100.5(3) . . . . ?
N13 Os1 O2 C3 172.6(3) . . . . ?
N11 Os1 O2 C3 34.3(17) . . . . ?
O1 Os1 O2 C3 -8.1(3) . . . . ?
P2 Os1 O2 C3 84.7(3) . . . . ?
P1 Os1 O2 C3 -90.9(3) . . . . ?
N13 Os1 N11 C11 -177.7(6) . . . . ?
O1 Os1 N11 C11 3.4(5) . . . . ?
O2 Os1 N11 C11 -38.2(19) . . . . ?
P2 Os1 N11 C11 -88.4(5) . . . . ?
P1 Os1 N11 C11 87.0(5) . . . . ?
N13 Os1 N11 C15 -1.6(4) . . . . ?
O1 Os1 N11 C15 179.5(4) . . . . ?
O2 Os1 N11 C15 137.9(15) . . . . ?
P2 Os1 N11 C15 87.7(4) . . . . ?
P1 Os1 N11 C15 -96.9(4) . . . . ?
C15 N12 N13 C16 179.9(5) . . . . ?
C15 N12 N13 Os1 -0.1(7) . . . . ?
N11 Os1 N13 N12 1.0(4) . . . . ?
O1 Os1 N13 N12 14(2) . . . . ?
O2 Os1 N13 N12 -174.6(4) . . . . ?
P2 Os1 N13 N12 -89.7(4) . . . . ?
P1 Os1 N13 N12 91.2(4) . . . . ?
N11 Os1 N13 C16 -179.1(5) . . . . ?
O1 Os1 N13 C16 -166.2(17) . . . . ?
O2 Os1 N13 C16 5.3(5) . . . . ?
P2 Os1 N13 C16 90.3(5) . . . . ?
P1 Os1 N13 C16 -88.9(5) . . . . ?
Os1 O1 C2 C1 178.3(4) . . . . ?
Os1 O1 C2 C3 -4.2(5) . . . . ?
C6 C1 C2 O1 -176.1(5) . . . . ?
Cl1 C1 C2 O1 0.0(8) . . . . ?
C6 C1 C2 C3 6.6(8) . . . . ?
Cl1 C1 C2 C3 -177.3(4) . . . . ?
Os1 O2 C3 C4 -172.2(4) . . . . ?
Os1 O2 C3 C2 8.5(6) . . . . ?
O1 C2 C3 O2 -3.0(7) . . . . ?
C1 C2 C3 O2 174.6(5) . . . . ?
O1 C2 C3 C4 177.6(5) . . . . ?
C1 C2 C3 C4 -4.8(8) . . . . ?
O2 C3 C4 C5 -177.8(6) . . . . ?
C2 C3 C4 C5 1.5(9) . . . . ?
O2 C3 C4 Cl2 -0.6(8) . . . . ?
C2 C3 C4 Cl2 178.8(4) . . . . ?
O10 O3 C5 C4 -174.4(5) . . . . ?
O10 O3 C5 C6 6.6(10) . . . . ?
C3 C4 C5 O3 -179.0(7) . . . . ?
Cl2 C4 C5 O3 3.7(10) . . . . ?
C3 C4 C5 C6 -0.1(9) . . . . ?
Cl2 C4 C5 C6 -177.4(5) . . . . ?
O10 O4 C6 C1 173.6(5) . . . . ?
O10 O4 C6 C5 -5.0(8) . . . . ?
C2 C1 C6 O4 176.5(6) . . . . ?
Cl1 C1 C6 O4 0.4(9) . . . . ?
C2 C1 C6 C5 -4.9(9) . . . . ?
Cl1 C1 C6 C5 179.0(4) . . . . ?
O3 C5 C6 O4 -0.7(10) . . . . ?
C4 C5 C6 O4 -179.7(6) . . . . ?
O3 C5 C6 C1 -179.4(6) . . . . ?
C4 C5 C6 C1 1.6(9) . . . . ?
C15 N11 C11 C12 1.7(10) . . . . ?
Os1 N11 C11 C12 177.7(5) . . . . ?
N11 C11 C12 C13 -0.6(12) . . . . ?
C11 C12 C13 C14 -1.1(14) . . . . ?
C12 C13 C14 C15 1.5(14) . . . . ?
C11 N11 C15 N12 178.6(6) . . . . ?
Os1 N11 C15 N12 2.1(8) . . . . ?
C11 N11 C15 C14 -1.2(10) . . . . ?
Os1 N11 C15 C14 -177.8(5) . . . . ?
N13 N12 C15 N11 -1.3(9) . . . . ?
N13 N12 C15 C14 178.6(6) . . . . ?
C13 C14 C15 N11 -0.3(12) . . . . ?
C13 C14 C15 N12 179.8(8) . . . . ?
N12 N13 C16 C21 -151.5(6) . . . . ?
Os1 N13 C16 C21 28.5(8) . . . . ?
N12 N13 C16 C17 27.6(9) . . . . ?
Os1 N13 C16 C17 -152.4(6) . . . . ?
C21 C16 C17 C18 -0.6(15) . . . . ?
N13 C16 C17 C18 -179.7(10) . . . . ?
C16 C17 C18 C19 -1(3) . . . . ?
C17 C18 C19 C20 2(3) . . . . ?
C18 C19 C20 C21 -3(3) . . . . ?
C17 C16 C21 C20 -0.3(12) . . . . ?
N13 C16 C21 C20 178.8(7) . . . . ?
C19 C20 C21 C16 2.1(16) . . . . ?
C41 P1 C31 C36 -115.3(5) . . . . ?
C51 P1 C31 C36 -3.6(6) . . . . ?
Os1 P1 C31 C36 119.9(5) . . . . ?
C41 P1 C31 C32 68.3(5) . . . . ?
C51 P1 C31 C32 -180.0(4) . . . . ?
Os1 P1 C31 C32 -56.4(5) . . . . ?
C36 C31 C32 C33 0.6(9) . . . . ?
P1 C31 C32 C33 177.2(5) . . . . ?
C31 C32 C33 C34 -2.2(10) . . . . ?
C32 C33 C34 C35 2.0(11) . . . . ?
C33 C34 C35 C36 -0.4(11) . . . . ?
C34 C35 C36 C31 -1.1(10) . . . . ?
C32 C31 C36 C35 1.0(9) . . . . ?
P1 C31 C36 C35 -175.3(5) . . . . ?
C51 P1 C41 C46 -113.9(5) . . . . ?
C31 P1 C41 C46 -1.6(6) . . . . ?
Os1 P1 C41 C46 121.6(5) . . . . ?
C51 P1 C41 C42 68.6(5) . . . . ?
C31 P1 C41 C42 -179.0(4) . . . . ?
Os1 P1 C41 C42 -55.9(5) . . . . ?
C46 C41 C42 C43 -1.4(9) . . . . ?
P1 C41 C42 C43 176.2(5) . . . . ?
C41 C42 C43 C44 -0.1(9) . . . . ?
C42 C43 C44 C45 1.7(10) . . . . ?
C43 C44 C45 C46 -2.1(11) . . . . ?
C44 C45 C46 C41 0.7(11) . . . . ?
C42 C41 C46 C45 1.0(9) . . . . ?
P1 C41 C46 C45 -176.4(5) . . . . ?
C41 P1 C51 C56 -10.9(6) . . . . ?
C31 P1 C51 C56 -122.7(5) . . . . ?
Os1 P1 C51 C56 114.5(5) . . . . ?
C41 P1 C51 C52 176.1(4) . . . . ?
C31 P1 C51 C52 64.3(5) . . . . ?
Os1 P1 C51 C52 -58.5(5) . . . . ?
C56 C51 C52 C53 -0.9(9) . . . . ?
P1 C51 C52 C53 172.3(5) . . . . ?
C51 C52 C53 C54 -0.6(10) . . . . ?
C52 C53 C54 C55 1.2(11) . . . . ?
C53 C54 C55 C56 -0.2(11) . . . . ?
C54 C55 C56 C51 -1.4(10) . . . . ?
C52 C51 C56 C55 1.9(9) . . . . ?
P1 C51 C56 C55 -171.1(5) . . . . ?
C81 P2 C61 C66 -12.7(5) . . . . ?
C71 P2 C61 C66 -121.2(5) . . . . ?
Os1 P2 C61 C66 115.6(5) . . . . ?
C81 P2 C61 C62 173.9(4) . . . . ?
C71 P2 C61 C62 65.4(5) . . . . ?
Os1 P2 C61 C62 -57.8(5) . . . . ?
C66 C61 C62 C63 1.6(8) . . . . ?
P2 C61 C62 C63 175.1(4) . . . . ?
C61 C62 C63 C64 -1.6(9) . . . . ?
C62 C63 C64 C65 -0.3(11) . . . . ?
C63 C64 C65 C66 2.1(12) . . . . ?
C64 C65 C66 C61 -2.1(11) . . . . ?
C62 C61 C66 C65 0.2(9) . . . . ?
P2 C61 C66 C65 -173.2(5) . . . . ?
C81 P2 C71 C76 -133.9(5) . . . . ?
C61 P2 C71 C76 -24.0(6) . . . . ?
Os1 P2 C71 C76 98.9(5) . . . . ?
C81 P2 C71 C72 50.8(5) . . . . ?
C61 P2 C71 C72 160.6(5) . . . . ?
Os1 P2 C71 C72 -76.5(5) . . . . ?
C76 C71 C72 C73 -2.6(9) . . . . ?
P2 C71 C72 C73 172.9(5) . . . . ?
C71 C72 C73 C74 1.6(11) . . . . ?
C72 C73 C74 C75 0.8(11) . . . . ?
C73 C74 C75 C76 -2.2(11) . . . . ?
C72 C71 C76 C75 1.4(9) . . . . ?
P2 C71 C76 C75 -174.0(5) . . . . ?
C74 C75 C76 C71 1.1(10) . . . . ?
C71 P2 C81 C86 -147.7(5) . . . . ?
C61 P2 C81 C86 100.2(5) . . . . ?
Os1 P2 C81 C86 -24.2(6) . . . . ?
C71 P2 C81 C82 34.7(5) . . . . ?
C61 P2 C81 C82 -77.4(5) . . . . ?
Os1 P2 C81 C82 158.2(4) . . . . ?
C86 C81 C82 C83 -0.3(9) . . . . ?
P2 C81 C82 C83 177.4(5) . . . . ?
C81 C82 C83 C84 1.3(10) . . . . ?
C82 C83 C84 C85 -1.5(11) . . . . ?
C83 C84 C85 C86 0.9(11) . . . . ?
C82 C81 C86 C85 -0.4(9) . . . . ?
P2 C81 C86 C85 -178.0(5) . . . . ?
C84 C85 C86 C81 0.1(11) . . . . ?
C5 O3 O10 O4 -6.3(6) . . . . ?
C6 O4 O10 O3 5.4(5) . . . . ?
