#------------------------------------------------------------------------------
#$Date: 2020-11-06 14:13:21 +0200 (Fri, 06 Nov 2020) $
#$Revision: 258835 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/54/7705486.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_7705486
loop_
_publ_author_name
'Parker, Amie'
'Lamata, Pilar'
'Viguri, Fernando'
'Rodríguez, Ricardo'
'López, José A'
'Lahoz, Fernando J.'
'García-Orduña, Pilar'
'Carmona, Daniel'
_publ_section_title
;
 Half-sandwich complexes of osmium containing guanidine-derived ligands.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13601
_journal_page_last               13617
_journal_paper_doi               10.1039/d0dt02713h
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C31 H38 N4 O Os, 2(F6 Sb), 2(C H2 Cl2)'
_chemical_formula_sum            'C33 H42 Cl4 F12 N4 O Os Sb2'
_chemical_formula_weight         1314.20
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   'Fourier Difference Synthesis'
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2020-07-31 deposited with the CCDC.	2020-09-17 downloaded from the CCDC.
;
_cell_angle_alpha                110.1590(10)
_cell_angle_beta                 92.3050(10)
_cell_angle_gamma                98.7480(10)
_cell_formula_units_Z            2
_cell_length_a                   8.709(8)
_cell_length_b                   15.2562(14)
_cell_length_c                   17.6428(16)
_cell_measurement_reflns_used    4367
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.970
_cell_measurement_theta_min      2.378
_cell_volume                     2164(2)
_computing_cell_refinement
'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_data_collection       'SMART in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_data_reduction
'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_molecular_graphics    'XP program, SHELXTL v6.12, Bruker2000'
_computing_publication_material  'XCIF program, PLATON(Spek, 1998)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       'narrow ω 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  0.0627
_diffrn_reflns_av_unetI/netI     0.0959
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22268
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.156
_diffrn_reflns_theta_min         2.210
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.499
_exptl_absorpt_correction_T_max  0.6240
_exptl_absorpt_correction_T_min  0.4359
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS 
 within APEX2 package.

;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.017
_exptl_crystal_description       prism
_exptl_crystal_F_000             1260
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane/hexane'
_exptl_crystal_size_max          0.165
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.110
_refine_diff_density_max         2.354
_refine_diff_density_min         -2.100
_refine_diff_density_rms         0.233
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     531
_refine_ls_number_reflns         9848
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.1011
_refine_ls_R_factor_gt           0.0636
_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)+(0.0486P)²+10.8565P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1225
_refine_ls_wR_factor_ref         0.1383
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6988
_reflns_number_total             9848
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt02713h2.cif
_cod_data_source_block           cmpnd_4
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_primary' value 'Direct method' was
changed to 'direct'.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7705482--7705488.cif.
;
_cod_database_code               7705486
_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.
;
_shelxl_version_number           2014-3
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 0.73024(4) 0.87424(3) 0.68078(2) 0.01902(11) Uani 1 1 d . . . . .
O O 0.9402(8) 0.8120(5) 0.6745(4) 0.0230(14) Uani 1 1 d D . . . .
N1 N 0.8846(9) 0.9981(6) 0.7430(5) 0.0235(18) Uani 1 1 d . . . . .
N2 N 0.7568(8) 0.8710(5) 0.7980(4) 0.0174(16) Uani 1 1 d . . . . .
N3 N 0.7241(10) 0.7095(6) 0.7629(5) 0.0228(17) Uani 1 1 d D . . . .
H3N H 0.780(10) 0.713(7) 0.724(4) 0.027 Uiso 1 1 d D U . . .
N4 N 0.6955(9) 0.8059(6) 0.8969(4) 0.0199(16) Uani 1 1 d D . . . .
C1 C 0.6001(12) 0.7545(8) 0.5787(6) 0.029(2) Uani 1 1 d . . . . .
C2 C 0.5055(11) 0.7809(7) 0.6390(6) 0.026(2) Uani 1 1 d . . . . .
H2 H 0.4524 0.7334 0.6566 0.031 Uiso 1 1 calc R U . . .
C3 C 0.4820(11) 0.8747(7) 0.6768(6) 0.024(2) Uani 1 1 d . . . . .
H3 H 0.4181 0.8894 0.7203 0.029 Uiso 1 1 calc R U . . .
C4 C 0.5540(10) 0.9483(7) 0.6498(6) 0.022(2) Uani 1 1 d . . . . .
C5 C 0.6462(11) 0.9206(8) 0.5836(6) 0.027(2) Uani 1 1 d . . . . .
H5 H 0.6928 0.9668 0.5627 0.032 Uiso 1 1 calc R U . . .
C6 C 0.6699(11) 0.8260(8) 0.5483(6) 0.030(2) Uani 1 1 d . . . . .
H6 H 0.7323 0.8095 0.5042 0.036 Uiso 1 1 calc R U . . .
C7 C 0.6332(13) 0.6561(8) 0.5411(7) 0.039(3) Uani 1 1 d . . . . .
H7A H 0.6062 0.6205 0.5769 0.058 Uiso 1 1 calc R U . . .
H7B H 0.7443 0.6591 0.5332 0.058 Uiso 1 1 calc R U . . .
H7C H 0.5707 0.6244 0.4885 0.058 Uiso 1 1 calc R U . . .
C8 C 0.5369(12) 1.0505(7) 0.6889(6) 0.029(2) Uani 1 1 d . . . . .
H8 H 0.6410 1.0901 0.6918 0.035 Uiso 1 1 calc R U . . .
C9 C 0.4247(13) 1.0737(8) 0.6341(6) 0.035(3) Uani 1 1 d . . . . .
H9A H 0.4626 1.0600 0.5804 0.053 Uiso 1 1 calc R U . . .
H9B H 0.4173 1.1410 0.6573 0.053 Uiso 1 1 calc R U . . .
H9C H 0.3215 1.0350 0.6290 0.053 Uiso 1 1 calc R U . . .
C10 C 0.4901(14) 1.0763(8) 0.7749(6) 0.038(3) Uani 1 1 d . . . . .
H10A H 0.3910 1.0361 0.7749 0.057 Uiso 1 1 calc R U . . .
H10B H 0.4779 1.1431 0.7955 0.057 Uiso 1 1 calc R U . . .
H10C H 0.5712 1.0665 0.8098 0.057 Uiso 1 1 calc R U . . .
C11 C 0.9716(10) 1.0518(7) 0.7077(6) 0.024(2) Uani 1 1 d . . . . .
H11 H 0.9649 1.0303 0.6501 0.029 Uiso 1 1 calc R U . . .
C12 C 1.0696(11) 1.1361(8) 0.7512(7) 0.031(2) Uani 1 1 d . . . . .
H12 H 1.1271 1.1729 0.7245 0.037 Uiso 1 1 calc R U . . .
C13 C 1.0810(12) 1.1653(8) 0.8350(7) 0.031(2) Uani 1 1 d . . . . .
H13 H 1.1483 1.2225 0.8669 0.037 Uiso 1 1 calc R U . . .
C14 C 0.9945(12) 1.1109(7) 0.8721(6) 0.030(2) Uani 1 1 d . . . . .
H14 H 1.0015 1.1303 0.9296 0.036 Uiso 1 1 calc R U . . .
C15 C 0.8977(10) 1.0278(7) 0.8244(6) 0.021(2) Uani 1 1 d . . . . .
C16 C 0.8013(12) 0.9666(7) 0.8614(6) 0.025(2) Uani 1 1 d . . . . .
H16A H 0.8622 0.9631 0.9086 0.030 Uiso 1 1 calc R U . . .
H16B H 0.7068 0.9931 0.8801 0.030 Uiso 1 1 calc R U . . .
C17 C 0.7237(10) 0.7963(7) 0.8192(6) 0.022(2) Uani 1 1 d . . . . .
C18 C 0.6218(11) 0.6229(7) 0.7505(6) 0.022(2) Uani 1 1 d . . . . .
C19 C 0.6641(12) 0.5392(7) 0.7017(6) 0.030(2) Uani 1 1 d . . . . .
H19 H 0.7606 0.5411 0.6785 0.036 Uiso 1 1 calc R U . . .
C20 C 0.5685(12) 0.4536(7) 0.6863(6) 0.030(2) Uani 1 1 d . . . . .
H20 H 0.5980 0.3975 0.6508 0.036 Uiso 1 1 calc R U . . .
C21 C 0.4269(13) 0.4471(8) 0.7221(7) 0.034(3) Uani 1 1 d . . . . .
C22 C 0.3893(11) 0.5312(8) 0.7700(6) 0.028(2) Uani 1 1 d . . . . .
H22 H 0.2946 0.5294 0.7947 0.033 Uiso 1 1 calc R U . . .
C23 C 0.4807(11) 0.6185(7) 0.7845(6) 0.026(2) Uani 1 1 d . . . . .
H23 H 0.4479 0.6749 0.8173 0.031 Uiso 1 1 calc R U . . .
C24 C 0.3311(15) 0.3526(9) 0.7082(9) 0.054(4) Uani 1 1 d . . . . .
H24A H 0.3658 0.3280 0.7493 0.080 Uiso 1 1 calc R U . . .
H24B H 0.3433 0.3087 0.6541 0.080 Uiso 1 1 calc R U . . .
H24C H 0.2210 0.3587 0.7122 0.080 Uiso 1 1 calc R U . . .
C25 C 0.7040(11) 0.7395(7) 0.9356(6) 0.024(2) Uani 1 1 d . . . . .
C26 C 0.8205(11) 0.6832(7) 0.9232(6) 0.025(2) Uani 1 1 d . . . . .
H26 H 0.8981 0.6890 0.8880 0.031 Uiso 1 1 calc R U . . .
C27 C 0.8212(12) 0.6194(7) 0.9625(6) 0.029(2) Uani 1 1 d . . . . .
H27 H 0.8986 0.5802 0.9527 0.034 Uiso 1 1 calc R U . . .
C28 C 0.7116(13) 0.6105(8) 1.0162(6) 0.032(3) Uani 1 1 d . . . . .
C29 C 0.5982(12) 0.6673(8) 1.0280(7) 0.035(3) Uani 1 1 d . . . . .
H29 H 0.5219 0.6626 1.0640 0.042 Uiso 1 1 calc R U . . .
C30 C 0.5947(11) 0.7309(7) 0.9877(6) 0.027(2) Uani 1 1 d . . . . .
H30 H 0.5157 0.7690 0.9964 0.032 Uiso 1 1 calc R U . . .
C31 C 0.7152(15) 0.5421(8) 1.0608(7) 0.044(3) Uani 1 1 d . . . . .
H31A H 0.7802 0.5740 1.1126 0.066 Uiso 1 1 calc R U . . .
H31B H 0.7588 0.4874 1.0278 0.066 Uiso 1 1 calc R U . . .
H31C H 0.6088 0.5205 1.0710 0.066 Uiso 1 1 calc R U . . .
Sb1 Sb 0.75551(7) 0.11011(5) 0.09632(4) 0.02318(16) Uani 1 1 d . . . . .
F1 F 0.6644(7) 0.1210(5) 0.0029(4) 0.0378(15) Uani 1 1 d . . . . .
F2 F 0.8456(6) 0.1011(5) 0.1924(3) 0.0342(14) Uani 1 1 d . . . . .
F3 F 0.8015(9) 0.2404(5) 0.1435(4) 0.0535(19) Uani 1 1 d . . . . .
F4 F 0.7117(7) -0.0213(4) 0.0501(4) 0.0360(14) Uani 1 1 d . . . . .
F5 F 0.5646(7) 0.1105(5) 0.1402(4) 0.0401(16) Uani 1 1 d . . . . .
F6 F 0.9484(6) 0.1086(5) 0.0545(4) 0.0365(15) Uani 1 1 d . . . . .
Sb2 Sb 0.12985(8) 0.79281(5) 0.44926(5) 0.03193(18) Uani 1 1 d . . . . .
F7 F 0.1428(12) 0.7724(7) 0.3396(5) 0.087(3) Uani 1 1 d . . . . .
F8 F 0.1211(10) 0.8172(7) 0.5595(5) 0.078(3) Uani 1 1 d . . . . .
F9A F 0.2913(18) 0.9001(9) 0.4740(8) 0.044(4) Uiso 0.60(2) 1 d . . P A 1
F10A F -0.0346(16) 0.6976(9) 0.4418(9) 0.049(4) Uiso 0.60(2) 1 d . . P A 1
F11A F -0.0134(17) 0.8775(12) 0.4636(10) 0.058(4) Uiso 0.60(2) 1 d . . P A 1
F12A F 0.3094(17) 0.7404(11) 0.4571(8) 0.044(4) Uiso 0.60(2) 1 d . . P A 1
F9B F 0.232(4) 0.9085(19) 0.4672(17) 0.080(9) Uiso 0.40(2) 1 d . . P A 2
F10B F 0.019(3) 0.6695(16) 0.4098(15) 0.063(7) Uiso 0.40(2) 1 d . . P A 2
F11B F -0.053(2) 0.8352(15) 0.4300(13) 0.040(5) Uiso 0.40(2) 1 d . . P A 2
F12B F 0.260(2) 0.7082(14) 0.4401(11) 0.033(5) Uiso 0.40(2) 1 d . . P A 2
C51 C 0.1652(15) 0.5297(8) 0.5999(7) 0.043(3) Uani 1 1 d . . . . .
H51A H 0.2564 0.5106 0.6214 0.051 Uiso 1 1 calc R U . . .
H51B H 0.0795 0.4741 0.5815 0.051 Uiso 1 1 calc R U . . .
Cl1 Cl 0.2147(4) 0.5621(2) 0.5172(2) 0.0493(8) Uani 1 1 d . . . . .
Cl2 Cl 0.1066(4) 0.6213(2) 0.6776(2) 0.0516(8) Uani 1 1 d . . . . .
C52 C 0.2172(15) 0.6108(11) 0.1903(9) 0.058(4) Uani 1 1 d . . . . .
H52A H 0.2688 0.6603 0.2414 0.070 Uiso 1 1 calc R U . . .
H52B H 0.2916 0.5677 0.1679 0.070 Uiso 1 1 calc R U . . .
Cl3 Cl 0.0478(4) 0.5451(3) 0.2120(2) 0.0692(11) Uani 1 1 d . . . . .
Cl4 Cl 0.1729(5) 0.6641(3) 0.1217(3) 0.0804(13) Uani 1 1 d . . . . .
H0A H 0.994(16) 0.792(11) 0.636(6) 0.10(6) Uiso 1 1 d D . . . .
H0B H 1.015(10) 0.834(8) 0.711(5) 0.05(4) Uiso 1 1 d D . . . .
H4N H 0.671(12) 0.860(4) 0.925(5) 0.03(3) Uiso 1 1 d 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Os N2 76.8(3) . . ?
N1 Os C3 119.7(3) . . ?
N2 Os C3 96.2(3) . . ?
N1 Os C2 157.2(3) . . ?
N2 Os C2 98.9(3) . . ?
C3 Os C2 37.9(4) . . ?
N1 Os O 82.7(3) . . ?
N2 Os O 79.7(3) . . ?
C3 Os O 156.0(3) . . ?
C2 Os O 118.9(3) . . ?
N1 Os C1 159.7(3) . . ?
N2 Os C1 122.5(3) . . ?
C3 Os C1 68.1(4) . . ?
C2 Os C1 36.3(4) . . ?
O Os C1 93.9(3) . . ?
N1 Os C4 93.7(3) . . ?
N2 Os C4 119.7(3) . . ?
C3 Os C4 38.4(3) . . ?
C2 Os C4 68.7(4) . . ?
O Os C4 159.1(3) . . ?
C1 Os C4 82.3(4) . . ?
N1 Os C5 96.2(3) . . ?
N2 Os C5 156.7(3) . . ?
C3 Os C5 67.7(4) . . ?
C2 Os C5 78.9(4) . . ?
O Os C5 121.9(3) . . ?
C1 Os C5 68.5(4) . . ?
C4 Os C5 37.7(3) . . ?
N1 Os C6 121.9(4) . . ?
N2 Os C6 160.3(3) . . ?
C3 Os C6 79.9(4) . . ?
C2 Os C6 66.2(4) . . ?
O Os C6 96.0(3) . . ?
C1 Os C6 38.2(4) . . ?
C4 Os C6 68.4(4) . . ?
C5 Os C6 37.3(4) . . ?
Os O H0A 131(10) . . ?
Os O H0B 122(9) . . ?
H0A O H0B 96(10) . . ?
C15 N1 C11 118.0(8) . . ?
C15 N1 Os 117.4(6) . . ?
C11 N1 Os 124.7(6) . . ?
C17 N2 C16 119.7(7) . . ?
C17 N2 Os 126.7(6) . . ?
C16 N2 Os 113.2(5) . . ?
C17 N3 C18 128.5(8) . . ?
C17 N3 H3N 112(7) . . ?
C18 N3 H3N 118(7) . . ?
C17 N4 C25 127.7(8) . . ?
C17 N4 H4N 114(7) . . ?
C25 N4 H4N 118(7) . . ?
C2 C1 C6 117.3(10) . . ?
C2 C1 C7 124.4(10) . . ?
C6 C1 C7 118.3(10) . . ?
C2 C1 Os 71.0(6) . . ?
C6 C1 Os 71.5(6) . . ?
C7 C1 Os 129.2(7) . . ?
C1 C2 C3 123.8(10) . . ?
C1 C2 Os 72.7(6) . . ?
C3 C2 Os 70.7(6) . . ?
C1 C2 H2 118.1 . . ?
C3 C2 H2 118.1 . . ?
Os C2 H2 131.7 . . ?
C2 C3 C4 120.2(9) . . ?
C2 C3 Os 71.4(6) . . ?
C4 C3 Os 72.0(5) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
Os C3 H3 129.0 . . ?
C5 C4 C3 116.6(9) . . ?
C5 C4 C8 120.5(9) . . ?
C3 C4 C8 122.9(9) . . ?
C5 C4 Os 71.6(5) . . ?
C3 C4 Os 69.5(5) . . ?
C8 C4 Os 128.7(6) . . ?
C6 C5 C4 121.6(9) . . ?
C6 C5 Os 71.5(5) . . ?
C4 C5 Os 70.7(5) . . ?
C6 C5 H5 119.2 . . ?
C4 C5 H5 119.2 . . ?
Os C5 H5 131.6 . . ?
C5 C6 C1 120.3(10) . . ?
C5 C6 Os 71.2(5) . . ?
C1 C6 Os 70.3(6) . . ?
C5 C6 H6 119.8 . . ?
C1 C6 H6 119.8 . . ?
Os C6 H6 131.5 . . ?
C1 C7 H7A 109.5 . . ?
C1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C4 C8 C9 108.6(8) . . ?
C4 C8 C10 114.3(8) . . ?
C9 C8 C10 112.0(9) . . ?
C4 C8 H8 107.2 . . ?
C9 C8 H8 107.2 . . ?
C10 C8 H8 107.2 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 C12 123.2(9) . . ?
N1 C11 H11 118.4 . . ?
C12 C11 H11 118.4 . . ?
C11 C12 C13 117.7(9) . . ?
C11 C12 H12 121.2 . . ?
C13 C12 H12 121.2 . . ?
C14 C13 C12 119.8(10) . . ?
C14 C13 H13 120.1 . . ?
C12 C13 H13 120.1 . . ?
C15 C14 C13 119.0(10) . . ?
C15 C14 H14 120.5 . . ?
C13 C14 H14 120.5 . . ?
N1 C15 C14 122.2(9) . . ?
N1 C15 C16 116.6(8) . . ?
C14 C15 C16 121.1(9) . . ?
N2 C16 C15 107.2(8) . . ?
N2 C16 H16A 110.3 . . ?
C15 C16 H16A 110.3 . . ?
N2 C16 H16B 110.3 . . ?
C15 C16 H16B 110.3 . . ?
H16A C16 H16B 108.5 . . ?
N2 C17 N3 118.4(8) . . ?
N2 C17 N4 120.9(9) . . ?
N3 C17 N4 120.6(8) . . ?
C19 C18 C23 118.7(9) . . ?
C19 C18 N3 118.3(9) . . ?
C23 C18 N3 123.0(9) . . ?
C20 C19 C18 120.8(10) . . ?
C20 C19 H19 119.6 . . ?
C18 C19 H19 119.6 . . ?
C19 C20 C21 121.4(10) . . ?
C19 C20 H20 119.3 . . ?
C21 C20 H20 119.3 . . ?
C22 C21 C20 116.0(10) . . ?
C22 C21 C24 124.1(11) . . ?
C20 C21 C24 119.9(10) . . ?
C21 C22 C23 123.9(10) . . ?
C21 C22 H22 118.1 . . ?
C23 C22 H22 118.1 . . ?
C22 C23 C18 119.2(9) . . ?
C22 C23 H23 120.4 . . ?
C18 C23 H23 120.4 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C30 C25 C26 119.2(9) . . ?
C30 C25 N4 118.4(9) . . ?
C26 C25 N4 122.3(9) . . ?
C27 C26 C25 119.3(9) . . ?
C27 C26 H26 120.4 . . ?
C25 C26 H26 120.4 . . ?
C26 C27 C28 122.0(10) . . ?
C26 C27 H27 119.0 . . ?
C28 C27 H27 119.0 . . ?
C29 C28 C27 117.7(9) . . ?
C29 C28 C31 120.5(10) . . ?
C27 C28 C31 121.8(10) . . ?
C28 C29 C30 120.9(10) . . ?
C28 C29 H29 119.6 . . ?
C30 C29 H29 119.6 . . ?
C25 C30 C29 120.8(10) . . ?
C25 C30 H30 119.6 . . ?
C29 C30 H30 119.6 . . ?
C28 C31 H31A 109.5 . . ?
C28 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C28 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
F3 Sb1 F4 179.0(3) . . ?
F3 Sb1 F6 90.4(3) . . ?
F4 Sb1 F6 89.2(3) . . ?
F3 Sb1 F5 89.9(3) . . ?
F4 Sb1 F5 90.4(3) . . ?
F6 Sb1 F5 178.5(3) . . ?
F3 Sb1 F1 89.9(3) . . ?
F4 Sb1 F1 91.0(3) . . ?
F6 Sb1 F1 90.8(3) . . ?
F5 Sb1 F1 90.7(3) . . ?
F3 Sb1 F2 89.2(3) . . ?
F4 Sb1 F2 89.9(3) . . ?
F6 Sb1 F2 90.1(2) . . ?
F5 Sb1 F2 88.5(2) . . ?
F1 Sb1 F2 178.8(3) . . ?
F9B Sb2 F12B 112.4(15) . . ?
F9B Sb2 F10B 169.0(12) . . ?
F12B Sb2 F10B 69.2(12) . . ?
F9B Sb2 F8 92.0(9) . . ?
F12B Sb2 F8 92.8(6) . . ?
F10A Sb2 F8 82.0(5) . . ?
F10B Sb2 F8 98.8(8) . . ?
F9B Sb2 F7 86.0(9) . . ?
F12B Sb2 F7 87.8(6) . . ?
F10A Sb2 F7 99.9(5) . . ?
F10B Sb2 F7 83.2(8) . . ?
F8 Sb2 F7 178.1(4) . . ?
F9B Sb2 F11B 87.8(11) . . ?
F12B Sb2 F11B 157.0(11) . . ?
F10B Sb2 F11B 88.8(9) . . ?
F8 Sb2 F11B 97.7(7) . . ?
F7 Sb2 F11B 82.4(7) . . ?
F10A Sb2 F12A 104.7(7) . . ?
F8 Sb2 F12A 87.5(5) . . ?
F7 Sb2 F12A 92.5(5) . . ?
F10A Sb2 F11A 88.8(6) . . ?
F8 Sb2 F11A 84.2(6) . . ?
F7 Sb2 F11A 95.3(6) . . ?
F12A Sb2 F11A 163.1(9) . . ?
F10A Sb2 F9A 170.9(6) . . ?
F8 Sb2 F9A 89.5(5) . . ?
F7 Sb2 F9A 88.6(5) . . ?
F12A Sb2 F9A 78.0(8) . . ?
F11A Sb2 F9A 87.2(6) . . ?
Cl1 C51 Cl2 112.5(6) . . ?
Cl1 C51 H51A 109.1 . . ?
Cl2 C51 H51A 109.1 . . ?
Cl1 C51 H51B 109.1 . . ?
Cl2 C51 H51B 109.1 . . ?
H51A C51 H51B 107.8 . . ?
Cl4 C52 Cl3 112.3(7) . . ?
Cl4 C52 H52A 109.1 . . ?
Cl3 C52 H52A 109.1 . . ?
Cl4 C52 H52B 109.1 . . ?
Cl3 C52 H52B 109.1 . . ?
H52A C52 H52B 107.9 . . ?
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 N1 2.064(8) . ?
Os N2 2.090(7) . ?
Os C3 2.162(10) . ?
Os C2 2.171(10) . ?
Os O 2.174(7) . ?
Os C1 2.193(10) . ?
Os C4 2.195(8) . ?
Os C5 2.206(8) . ?
Os C6 2.209(9) . ?
O H0A 0.84(2) . ?
O H0B 0.84(2) . ?
N1 C15 1.341(11) . ?
N1 C11 1.355(11) . ?
N2 C17 1.313(11) . ?
N2 C16 1.483(12) . ?
N3 C17 1.356(13) . ?
N3 C18 1.419(12) . ?
N3 H3N 0.87(2) . ?
N4 C17 1.363(11) . ?
N4 C25 1.412(11) . ?
N4 H4N 0.87(2) . ?
C1 C2 1.360(14) . ?
C1 C6 1.442(14) . ?
C1 C7 1.495(15) . ?
C2 C3 1.406(14) . ?
C2 H2 0.9500 . ?
C3 C4 1.435(13) . ?
C3 H3 0.9500 . ?
C4 C5 1.423(13) . ?
C4 C8 1.505(13) . ?
C5 C6 1.412(14) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.510(12) . ?
C8 C10 1.519(14) . ?
C8 H8 1.0000 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.380(14) . ?
C11 H11 0.9500 . ?
C12 C13 1.384(14) . ?
C12 H12 0.9500 . ?
C13 C14 1.382(14) . ?
C13 H13 0.9500 . ?
C14 C15 1.381(14) . ?
C14 H14 0.9500 . ?
C15 C16 1.493(12) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C18 C19 1.386(14) . ?
C18 C23 1.391(14) . ?
C19 C20 1.371(14) . ?
C19 H19 0.9500 . ?
C20 C21 1.413(15) . ?
C20 H20 0.9500 . ?
C21 C22 1.367(15) . ?
C21 C24 1.487(15) . ?
C22 C23 1.377(14) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C30 1.373(13) . ?
C25 C26 1.404(14) . ?
C26 C27 1.376(13) . ?
C26 H26 0.9500 . ?
C27 C28 1.397(15) . ?
C27 H27 0.9500 . ?
C28 C29 1.385(16) . ?
C28 C31 1.511(13) . ?
C29 C30 1.389(13) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
Sb1 F3 1.842(7) . ?
Sb1 F4 1.856(6) . ?
Sb1 F6 1.862(6) . ?
Sb1 F5 1.862(6) . ?
Sb1 F1 1.871(5) . ?
Sb1 F2 1.896(5) . ?
Sb2 F9B 1.77(3) . ?
Sb2 F12B 1.816(16) . ?
Sb2 F10A 1.843(12) . ?
Sb2 F10B 1.86(2) . ?
Sb2 F8 1.857(7) . ?
Sb2 F7 1.862(8) . ?
Sb2 F11B 1.871(17) . ?
Sb2 F12A 1.882(13) . ?
Sb2 F11A 1.893(14) . ?
Sb2 F9A 1.899(13) . ?
C51 Cl1 1.745(12) . ?
C51 Cl2 1.745(12) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 Cl4 1.736(13) . ?
C52 Cl3 1.786(14) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
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
C6 C1 C2 C3 -4.8(13) . . . . ?
C7 C1 C2 C3 176.5(9) . . . . ?
Os C1 C2 C3 51.4(8) . . . . ?
C6 C1 C2 Os -56.2(8) . . . . ?
C7 C1 C2 Os 125.1(9) . . . . ?
C1 C2 C3 C4 2.8(13) . . . . ?
Os C2 C3 C4 55.1(7) . . . . ?
C1 C2 C3 Os -52.2(8) . . . . ?
C2 C3 C4 C5 0.8(12) . . . . ?
Os C3 C4 C5 55.6(7) . . . . ?
C2 C3 C4 C8 -178.4(8) . . . . ?
Os C3 C4 C8 -123.6(8) . . . . ?
C2 C3 C4 Os -54.8(7) . . . . ?
C3 C4 C5 C6 -2.2(13) . . . . ?
C8 C4 C5 C6 177.1(8) . . . . ?
Os C4 C5 C6 52.4(8) . . . . ?
C3 C4 C5 Os -54.6(7) . . . . ?
C8 C4 C5 Os 124.7(8) . . . . ?
C4 C5 C6 C1 0.2(14) . . . . ?
Os C5 C6 C1 52.2(8) . . . . ?
C4 C5 C6 Os -52.0(8) . . . . ?
C2 C1 C6 C5 3.3(13) . . . . ?
C7 C1 C6 C5 -177.9(9) . . . . ?
Os C1 C6 C5 -52.7(8) . . . . ?
C2 C1 C6 Os 56.0(8) . . . . ?
C7 C1 C6 Os -125.3(8) . . . . ?
C5 C4 C8 C9 76.0(11) . . . . ?
C3 C4 C8 C9 -104.8(10) . . . . ?
Os C4 C8 C9 166.1(7) . . . . ?
C5 C4 C8 C10 -158.2(9) . . . . ?
C3 C4 C8 C10 21.0(13) . . . . ?
Os C4 C8 C10 -68.1(12) . . . . ?
C15 N1 C11 C12 -1.5(14) . . . . ?
Os N1 C11 C12 177.5(7) . . . . ?
N1 C11 C12 C13 1.6(15) . . . . ?
C11 C12 C13 C14 -0.8(15) . . . . ?
C12 C13 C14 C15 0.0(15) . . . . ?
C11 N1 C15 C14 0.7(13) . . . . ?
Os N1 C15 C14 -178.4(7) . . . . ?
C11 N1 C15 C16 -179.5(8) . . . . ?
Os N1 C15 C16 1.4(11) . . . . ?
C13 C14 C15 N1 0.0(15) . . . . ?
C13 C14 C15 C16 -179.8(9) . . . . ?
C17 N2 C16 C15 155.0(8) . . . . ?
Os N2 C16 C15 -31.6(9) . . . . ?
N1 C15 C16 N2 19.6(11) . . . . ?
C14 C15 C16 N2 -160.6(8) . . . . ?
C16 N2 C17 N3 -162.8(8) . . . . ?
Os N2 C17 N3 24.7(12) . . . . ?
C16 N2 C17 N4 14.8(13) . . . . ?
Os N2 C17 N4 -157.8(6) . . . . ?
C18 N3 C17 N2 -142.0(9) . . . . ?
C18 N3 C17 N4 40.4(13) . . . . ?
C25 N4 C17 N2 -159.7(9) . . . . ?
C25 N4 C17 N3 17.8(14) . . . . ?
C17 N3 C18 C19 -165.8(9) . . . . ?
C17 N3 C18 C23 14.9(14) . . . . ?
C23 C18 C19 C20 0.6(14) . . . . ?
N3 C18 C19 C20 -178.7(9) . . . . ?
C18 C19 C20 C21 -2.5(15) . . . . ?
C19 C20 C21 C22 2.4(15) . . . . ?
C19 C20 C21 C24 -176.1(10) . . . . ?
C20 C21 C22 C23 -0.3(14) . . . . ?
C24 C21 C22 C23 178.1(10) . . . . ?
C21 C22 C23 C18 -1.5(14) . . . . ?
C19 C18 C23 C22 1.4(13) . . . . ?
N3 C18 C23 C22 -179.3(8) . . . . ?
C17 N4 C25 C30 -141.8(10) . . . . ?
C17 N4 C25 C26 38.8(14) . . . . ?
C30 C25 C26 C27 1.1(14) . . . . ?
N4 C25 C26 C27 -179.6(9) . . . . ?
C25 C26 C27 C28 -1.7(15) . . . . ?
C26 C27 C28 C29 1.3(15) . . . . ?
C26 C27 C28 C31 -178.5(10) . . . . ?
C27 C28 C29 C30 -0.3(15) . . . . ?
C31 C28 C29 C30 179.5(10) . . . . ?
C26 C25 C30 C29 -0.1(15) . . . . ?
N4 C25 C30 C29 -179.5(9) . . . . ?
C28 C29 C30 C25 -0.3(16) . . . . ?
