#------------------------------------------------------------------------------
#$Date: 2019-11-28 19:03:14 +0200 (Thu, 28 Nov 2019) $
#$Revision: 244373 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/63/1556345.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_1556345
loop_
_publ_author_name
'Fu, Ying'
'Romero, María J.'
'Habtemariam, Abraha'
'Snowden, Michael E.'
'Song, Lijiang'
'Clarkson, Guy J.'
'Qamar, Bushra'
'Pizarro, Ana M.'
'Unwin, Patrick R.'
'Sadler, Peter J.'
_publ_section_title
;
 The contrasting chemical reactivity of potent isoelectronic iminopyridine
 and azopyridine osmium(ii) arene anticancer complexes
;
_journal_issue                   8
_journal_name_full               'Chemical Science'
_journal_page_first              2485
_journal_paper_doi               10.1039/c2sc20220d
_journal_volume                  3
_journal_year                    2012
_chemical_formula_sum            'C22.5 H27 Cl F6 I N2 O2 Os P'
_chemical_formula_weight         854.98
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                95.3980(19)
_cell_angle_beta                 103.654(2)
_cell_angle_gamma                97.2625(19)
_cell_formula_units_Z            4
_cell_length_a                   11.3168(3)
_cell_length_b                   13.0498(3)
_cell_length_c                   19.2278(4)
_cell_measurement_reflns_used    14468
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.29
_cell_measurement_theta_min      3.09
_cell_volume                     2714.50(12)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.2833
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.842
_diffrn_measurement_device_type  'Oxford Diffraction Gemini R'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0222
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24068
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         29.36
_diffrn_reflns_theta_min         3.10
_diffrn_standards_decay_%        nil
_exptl_absorpt_coefficient_mu    6.057
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.47
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSPACK(CrysAlis, Oxford Diffraction)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.092
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1628
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         4.429
_refine_diff_density_min         -1.365
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     728
_refine_ls_number_reflns         12572
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0440P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0817
_reflns_number_gt                9981
_reflns_number_total             12572
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2sc20220d.txt
_cod_data_source_block           fy20
_cod_original_cell_volume        2714.50(11)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C22.50 H27 Cl F6 I N2 O2 Os P'
_cod_database_code               1556345
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
Os1 Os 0.423688(17) 0.293385(13) 0.215743(9) 0.01272(5) Uani 1 1 d . . .
I1 I 0.66975(3) 0.34850(2) 0.237002(16) 0.01836(7) Uani 1 1 d . . .
N101 N 0.4683(4) 0.1513(3) 0.24693(19) 0.0139(8) Uani 1 1 d . . .
C102 C 0.4758(5) 0.0672(3) 0.2027(3) 0.0181(10) Uani 1 1 d . . .
H10A H 0.4555 0.0697 0.1521 0.022 Uiso 1 1 calc R . .
C103 C 0.5118(5) -0.0224(4) 0.2281(3) 0.0211(11) Uani 1 1 d . . .
H10B H 0.5155 -0.0803 0.1952 0.025 Uiso 1 1 calc R . .
C104 C 0.5425(5) -0.0274(4) 0.3017(3) 0.0231(11) Uani 1 1 d . . .
H10C H 0.5667 -0.0888 0.3200 0.028 Uiso 1 1 calc R . .
C105 C 0.5373(5) 0.0576(4) 0.3475(3) 0.0225(11) Uani 1 1 d . . .
H10D H 0.5599 0.0564 0.3982 0.027 Uiso 1 1 calc R . .
C106 C 0.4990(5) 0.1456(4) 0.3198(2) 0.0188(10) Uani 1 1 d . . .
C107 C 0.4887(5) 0.2398(4) 0.3622(2) 0.0205(11) Uani 1 1 d . . .
H10E H 0.5055 0.2458 0.4134 0.025 Uiso 1 1 calc R . .
N108 N 0.4556(4) 0.3158(3) 0.32742(19) 0.0173(9) Uani 1 1 d . . .
C109 C 0.4335(5) 0.4060(4) 0.3675(2) 0.0203(11) Uani 1 1 d . . .
C110 C 0.3630(5) 0.3952(4) 0.4178(3) 0.0259(12) Uani 1 1 d . . .
H11A H 0.3345 0.3278 0.4275 0.031 Uiso 1 1 calc R . .
C111 C 0.3348(5) 0.4813(4) 0.4531(3) 0.0278(12) Uani 1 1 d . . .
H11B H 0.2862 0.4735 0.4869 0.033 Uiso 1 1 calc R . .
C112 C 0.3769(5) 0.5790(4) 0.4395(3) 0.0272(12) Uani 1 1 d . . .
C113 C 0.4498(5) 0.5920(4) 0.3897(2) 0.0251(12) Uani 1 1 d . . .
H11C H 0.4803 0.6598 0.3814 0.030 Uiso 1 1 calc R . .
C114 C 0.4764(5) 0.5037(4) 0.3528(2) 0.0217(11) Uani 1 1 d . . .
H11D H 0.5233 0.5106 0.3181 0.026 Uiso 1 1 calc R . .
O115 O 0.3449(4) 0.6622(3) 0.47569(19) 0.0355(10) Uani 1 1 d . . .
H11H H 0.3664 0.7168 0.4591 0.053 Uiso 1 1 calc R . .
C116 C 0.2965(5) 0.4068(4) 0.1961(3) 0.0196(11) Uani 1 1 d . . .
H11E H 0.3002 0.4627 0.2362 0.023 Uiso 1 1 calc R . .
C117 C 0.3784(5) 0.4224(4) 0.1529(3) 0.0212(11) Uani 1 1 d . . .
H11F H 0.4380 0.4887 0.1629 0.025 Uiso 1 1 calc R . .
C118 C 0.3928(5) 0.3392(4) 0.1033(2) 0.0232(11) Uani 1 1 d . . .
C119 C 0.3256(5) 0.2411(4) 0.1011(2) 0.0195(11) Uani 1 1 d . . .
H11G H 0.3487 0.1794 0.0755 0.023 Uiso 1 1 calc R . .
C120 C 0.2437(5) 0.2236(4) 0.1470(2) 0.0171(10) Uani 1 1 d . . .
H12K H 0.2094 0.1506 0.1511 0.021 Uiso 1 1 calc R . .
C121 C 0.2262(5) 0.3072(4) 0.1948(2) 0.0189(10) Uani 1 1 d . . .
C122 C 0.1382(5) 0.2930(4) 0.2432(3) 0.0267(12) Uani 1 1 d . . .
H12J H 0.1703 0.3457 0.2871 0.032 Uiso 1 1 calc R . .
C123 C 0.0137(5) 0.3179(4) 0.2027(3) 0.0293(13) Uani 1 1 d . . .
H12A H 0.0253 0.3863 0.1861 0.044 Uiso 1 1 calc R . .
H12B H -0.0414 0.3188 0.2351 0.044 Uiso 1 1 calc R . .
H12C H -0.0226 0.2647 0.1611 0.044 Uiso 1 1 calc R . .
C124 C 0.1275(6) 0.1864(5) 0.2680(3) 0.0366(14) Uani 1 1 d . . .
H12D H 0.2098 0.1716 0.2904 0.055 Uiso 1 1 calc R . .
H12E H 0.0884 0.1336 0.2265 0.055 Uiso 1 1 calc R . .
H12F H 0.0775 0.1847 0.3033 0.055 Uiso 1 1 calc R . .
C125 C 0.4773(6) 0.3570(5) 0.0551(3) 0.0351(14) Uani 1 1 d . . .
H12G H 0.5199 0.2967 0.0510 0.053 Uiso 1 1 calc R . .
H12H H 0.5379 0.4195 0.0755 0.053 Uiso 1 1 calc R . .
H12I H 0.4295 0.3666 0.0072 0.053 Uiso 1 1 calc R . .
Os2 Os 0.885772(19) 0.739783(14) 0.253643(9) 0.01773(6) Uani 1 1 d . . .
I2 I 0.63770(3) 0.69529(2) 0.235262(18) 0.02308(8) Uani 1 1 d . . .
N201 N 0.8505(4) 0.8902(3) 0.2403(2) 0.0188(9) Uani 1 1 d . . .
C202 C 0.8541(5) 0.9663(4) 0.2936(3) 0.0258(12) Uani 1 1 d . . .
H20A H 0.8748 0.9528 0.3424 0.031 Uiso 1 1 calc R . .
C203 C 0.8279(5) 1.0645(4) 0.2783(3) 0.0291(13) Uani 1 1 d . . .
H20B H 0.8308 1.1170 0.3166 0.035 Uiso 1 1 calc R . .
C204 C 0.7979(5) 1.0861(4) 0.2081(3) 0.0278(12) Uani 1 1 d . . .
H20C H 0.7785 1.1526 0.1975 0.033 Uiso 1 1 calc R . .
C205 C 0.7965(5) 1.0090(4) 0.1531(3) 0.0254(12) Uani 1 1 d . . .
H20D H 0.7787 1.0223 0.1043 0.030 Uiso 1 1 calc R . .
C206 C 0.8213(5) 0.9129(4) 0.1707(3) 0.0200(10) Uani 1 1 d . . .
C207 C 0.8183(5) 0.8254(4) 0.1186(2) 0.0204(11) Uani 1 1 d . . .
H20E H 0.7985 0.8308 0.0684 0.025 Uiso 1 1 calc R . .
N208 N 0.8436(4) 0.7390(3) 0.1424(2) 0.0188(9) Uani 1 1 d . . .
C209 C 0.8429(5) 0.6508(4) 0.0912(2) 0.0194(11) Uani 1 1 d . . .
C210 C 0.7964(5) 0.5518(4) 0.0998(3) 0.0221(11) Uani 1 1 d . . .
H21A H 0.7677 0.5405 0.1415 0.027 Uiso 1 1 calc R . .
C211 C 0.7909(5) 0.4686(4) 0.0487(3) 0.0245(12) Uani 1 1 d . . .
H21B H 0.7591 0.4003 0.0554 0.029 Uiso 1 1 calc R . .
C212 C 0.8322(5) 0.4847(4) -0.0130(3) 0.0258(12) Uani 1 1 d . . .
C213 C 0.8833(5) 0.5827(4) -0.0207(3) 0.0270(13) Uani 1 1 d . . .
H21C H 0.9147 0.5928 -0.0616 0.032 Uiso 1 1 calc R . .
C214 C 0.8899(5) 0.6681(4) 0.0306(2) 0.0214(11) Uani 1 1 d . . .
H21D H 0.9251 0.7358 0.0249 0.026 Uiso 1 1 calc R . .
O215 O 0.8234(4) 0.4059(3) -0.0676(2) 0.0346(10) Uani 1 1 d . . .
H21H H 0.8003 0.3485 -0.0548 0.052 Uiso 1 1 calc R . .
C216 C 1.0175(5) 0.6313(4) 0.2523(3) 0.0220(11) Uani 1 1 d . . .
H21E H 1.0154 0.5899 0.2054 0.026 Uiso 1 1 calc R . .
C217 C 0.9362(5) 0.5937(4) 0.2931(3) 0.0263(12) Uani 1 1 d . . .
H21F H 0.8784 0.5271 0.2740 0.032 Uiso 1 1 calc R . .
C218 C 0.9185(5) 0.6586(4) 0.3528(3) 0.0256(12) Uani 1 1 d . . .
C219 C 0.9831(5) 0.7607(4) 0.3694(3) 0.0268(12) Uani 1 1 d . . .
H21G H 0.9585 0.8115 0.4035 0.032 Uiso 1 1 calc R . .
C220 C 1.0638(5) 0.7986(4) 0.3271(3) 0.0240(11) Uani 1 1 d . . .
H22K H 1.0948 0.8750 0.3335 0.029 Uiso 1 1 calc R . .
C221 C 1.0838(5) 0.7347(4) 0.2687(2) 0.0231(11) Uani 1 1 d . . .
C222 C 1.1654(5) 0.7729(4) 0.2208(3) 0.0255(12) Uani 1 1 d . . .
H22A H 1.1232 0.7425 0.1699 0.031 Uiso 1 1 calc R . .
C223 C 1.1853(6) 0.8905(4) 0.2232(3) 0.0348(14) Uani 1 1 d . . .
H22B H 1.1054 0.9149 0.2112 0.052 Uiso 1 1 calc R . .
H22C H 1.2318 0.9101 0.1882 0.052 Uiso 1 1 calc R . .
H22D H 1.2315 0.9224 0.2718 0.052 Uiso 1 1 calc R . .
C224 C 1.2892(6) 0.7319(5) 0.2409(3) 0.0365(14) Uani 1 1 d . . .
H22E H 1.2741 0.6566 0.2424 0.055 Uiso 1 1 calc R . .
H22F H 1.3370 0.7667 0.2885 0.055 Uiso 1 1 calc R . .
H22G H 1.3353 0.7463 0.2048 0.055 Uiso 1 1 calc R . .
C225 C 0.8312(6) 0.6203(5) 0.3951(3) 0.0351(14) Uani 1 1 d . . .
H22H H 0.7637 0.5701 0.3636 0.053 Uiso 1 1 calc R . .
H22I H 0.7979 0.6792 0.4147 0.053 Uiso 1 1 calc R . .
H22J H 0.8746 0.5865 0.4348 0.053 Uiso 1 1 calc R . .
P10 P 0.76477(17) 0.91261(11) 0.51875(8) 0.0334(4) Uani 1 1 d D . .
F11 F 0.7791(13) 0.9185(9) 0.4417(6) 0.067(3) Uani 0.431(8) 1 d PU A 1
F12 F 0.7267(17) 0.9214(13) 0.5925(8) 0.095(5) Uani 0.431(8) 1 d PU A 1
F13 F 0.8640(14) 0.8471(12) 0.5364(7) 0.082(4) Uani 0.431(8) 1 d PU A 1
F14 F 0.6381(10) 0.9733(8) 0.4957(5) 0.056(3) Uani 0.431(8) 1 d PU A 1
F15 F 0.8372(14) 1.0161(10) 0.5520(7) 0.086(4) Uani 0.431(8) 1 d PU A 1
F16 F 0.6615(11) 0.8060(9) 0.4807(7) 0.076(4) Uani 0.431(8) 1 d PU A 1
F11A F 0.8608(9) 0.9265(6) 0.4675(4) 0.067(2) Uani 0.569(8) 1 d PDU A 2
F12A F 0.6830(9) 0.8887(7) 0.5723(5) 0.062(3) Uani 0.569(8) 1 d PDU A 2
F13A F 0.8070(10) 0.8026(6) 0.5312(5) 0.064(2) Uani 0.569(8) 1 d PDU A 2
F14A F 0.7384(10) 1.0268(6) 0.5089(4) 0.070(3) Uani 0.569(8) 1 d PDU A 2
F15A F 0.8802(8) 0.9639(6) 0.5866(4) 0.066(3) Uani 0.569(8) 1 d PDU A 2
F16A F 0.6630(9) 0.8649(8) 0.4483(5) 0.088(3) Uani 0.569(8) 1 d PDU A 2
P20 P 0.5000 0.0000 0.0000 0.0271(5) Uani 1 2 d S . .
F21 F 0.5175(4) -0.0772(3) 0.06012(17) 0.0480(10) Uani 1 1 d . . .
F22 F 0.3734(3) 0.0208(3) 0.01686(18) 0.0452(9) Uani 1 1 d . . .
F23 F 0.5720(3) 0.0952(2) 0.05954(16) 0.0355(8) Uani 1 1 d . . .
P30 P 0.0000 0.0000 0.0000 0.0200(4) Uani 1 2 d S . .
F31 F 0.0303(4) -0.0289(3) 0.07957(18) 0.0582(11) Uani 1 1 d . . .
F32 F 0.1371(3) 0.0566(3) 0.01285(17) 0.0413(9) Uani 1 1 d . . .
F33 F -0.0388(4) 0.1056(3) 0.0287(2) 0.0619(12) Uani 1 1 d . . .
O300 O 0.7511(6) 0.2108(4) -0.0382(3) 0.0607(14) Uani 1 1 d D . .
H30A H 0.817(5) 0.186(7) -0.014(4) 0.091 Uiso 1 1 d D . .
H30B H 0.674(3) 0.177(6) -0.053(5) 0.091 Uiso 1 1 d D . .
O400 O 0.4042(5) 0.8452(3) 0.4313(2) 0.0529(13) Uani 1 1 d . . .
C500 C 0.8596(6) 0.3475(5) 0.4430(3) 0.0402(15) Uani 1 1 d . . .
H50A H 0.8697 0.3893 0.4903 0.048 Uiso 1 1 calc R . .
H50B H 0.7840 0.3620 0.4098 0.048 Uiso 1 1 calc R . .
Cl1 Cl 0.84330(17) 0.21679(13) 0.45317(8) 0.0459(4) Uani 1 1 d . . .
Cl2 Cl 0.99189(17) 0.38677(15) 0.40728(8) 0.0496(4) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N108 Os1 N101 76.05(14) . .
N108 Os1 C120 121.35(17) . .
N101 Os1 C120 93.60(16) . .
N108 Os1 C116 95.57(16) . .
N101 Os1 C116 151.92(18) . .
C120 Os1 C116 67.59(18) . .
N108 Os1 C117 119.97(16) . .
N101 Os1 C117 163.85(16) . .
C120 Os1 C117 79.85(18) . .
C116 Os1 C117 36.90(18) . .
N108 Os1 C121 95.02(16) . .
N101 Os1 C121 115.09(17) . .
C120 Os1 C121 37.83(17) . .
C116 Os1 C121 37.98(18) . .
C117 Os1 C121 68.07(19) . .
N108 Os1 C119 159.24(18) . .
N101 Os1 C119 99.42(16) . .
C120 Os1 C119 38.04(17) . .
C116 Os1 C119 78.86(17) . .
C117 Os1 C119 66.38(18) . .
C121 Os1 C119 68.21(17) . .
N108 Os1 C118 156.77(17) . .
N101 Os1 C118 126.56(16) . .
C120 Os1 C118 67.54(19) . .
C116 Os1 C118 66.91(18) . .
C117 Os1 C118 37.30(18) . .
C121 Os1 C118 80.52(18) . .
C119 Os1 C118 36.33(19) . .
N108 Os1 I1 86.38(12) . .
N101 Os1 I1 84.80(11) . .
C120 Os1 I1 151.06(12) . .
C116 Os1 I1 121.86(14) . .
C117 Os1 I1 93.79(14) . .
C121 Os1 I1 159.84(13) . .
C119 Os1 I1 113.65(13) . .
C118 Os1 I1 90.27(14) . .
C102 N101 C106 117.4(4) . .
C102 N101 Os1 126.2(3) . .
C106 N101 Os1 116.3(3) . .
N101 C102 C103 122.5(4) . .
N101 C102 H10A 118.8 . .
C103 C102 H10A 118.8 . .
C102 C103 C104 119.7(4) . .
C102 C103 H10B 120.1 . .
C104 C103 H10B 120.1 . .
C105 C104 C103 118.6(4) . .
C105 C104 H10C 120.7 . .
C103 C104 H10C 120.7 . .
C104 C105 C106 119.9(4) . .
C104 C105 H10D 120.0 . .
C106 C105 H10D 120.0 . .
N101 C106 C105 121.8(4) . .
N101 C106 C107 112.9(4) . .
C105 C106 C107 125.3(4) . .
N108 C107 C106 116.9(4) . .
N108 C107 H10E 121.5 . .
C106 C107 H10E 121.5 . .
C107 N108 C109 117.8(4) . .
C107 N108 Os1 117.7(3) . .
C109 N108 Os1 124.2(3) . .
C114 C109 C110 120.6(4) . .
C114 C109 N108 119.2(4) . .
C110 C109 N108 120.1(4) . .
C111 C110 C109 120.4(5) . .
C111 C110 H11A 119.8 . .
C109 C110 H11A 119.8 . .
C110 C111 C112 119.8(5) . .
C110 C111 H11B 120.1 . .
C112 C111 H11B 120.1 . .
O115 C112 C111 117.4(5) . .
O115 C112 C113 121.8(5) . .
C111 C112 C113 120.8(4) . .
C114 C113 C112 119.0(5) . .
C114 C113 H11C 120.5 . .
C112 C113 H11C 120.5 . .
C109 C114 C113 119.2(5) . .
C109 C114 H11D 120.4 . .
C113 C114 H11D 120.4 . .
C112 O115 H11H 109.5 . .
C117 C116 C121 122.2(4) . .
C117 C116 Os1 72.2(3) . .
C121 C116 Os1 71.8(3) . .
C117 C116 H11E 118.3 . .
C121 C116 H11E 118.3 . .
Os1 C116 H11E 118.3 . .
C116 C117 C118 120.8(5) . .
C116 C117 Os1 70.9(3) . .
C118 C117 Os1 73.3(3) . .
C116 C117 H11F 119.2 . .
C118 C117 H11F 119.2 . .
Os1 C117 H11F 119.2 . .
C119 C118 C117 118.2(4) . .
C119 C118 C125 121.1(5) . .
C117 C118 C125 120.7(5) . .
C119 C118 Os1 70.4(3) . .
C117 C118 Os1 69.4(3) . .
C125 C118 Os1 132.1(4) . .
C118 C119 C120 121.3(4) . .
C118 C119 Os1 73.3(3) . .
C120 C119 Os1 69.6(2) . .
C118 C119 H11G 118.6 . .
C120 C119 H11G 118.6 . .
Os1 C119 H11G 118.6 . .
C121 C120 C119 120.6(4) . .
C121 C120 Os1 72.1(3) . .
C119 C120 Os1 72.4(3) . .
C121 C120 H12K 119.3 . .
C119 C120 H12K 119.3 . .
Os1 C120 H12K 119.3 . .
C120 C121 C116 116.8(4) . .
C120 C121 C122 122.5(5) . .
C116 C121 C122 120.7(4) . .
C120 C121 Os1 70.0(3) . .
C116 C121 Os1 70.2(3) . .
C122 C121 Os1 130.1(3) . .
C124 C122 C121 113.3(4) . .
C124 C122 C123 112.2(5) . .
C121 C122 C123 107.9(4) . .
C124 C122 H12J 107.7 . .
C121 C122 H12J 107.7 . .
C123 C122 H12J 107.7 . .
C122 C123 H12A 109.5 . .
C122 C123 H12B 109.5 . .
H12A C123 H12B 109.5 . .
C122 C123 H12C 109.5 . .
H12A C123 H12C 109.5 . .
H12B C123 H12C 109.5 . .
C122 C124 H12D 109.5 . .
C122 C124 H12E 109.5 . .
H12D C124 H12E 109.5 . .
C122 C124 H12F 109.5 . .
H12D C124 H12F 109.5 . .
H12E C124 H12F 109.5 . .
C118 C125 H12G 109.5 . .
C118 C125 H12H 109.5 . .
H12G C125 H12H 109.5 . .
C118 C125 H12I 109.5 . .
H12G C125 H12I 109.5 . .
H12H C125 H12I 109.5 . .
N208 Os2 N201 76.59(15) . .
N208 Os2 C220 125.39(18) . .
N201 Os2 C220 91.36(18) . .
N208 Os2 C216 93.28(16) . .
N201 Os2 C216 145.64(18) . .
C220 Os2 C216 67.67(18) . .
N208 Os2 C221 96.74(17) . .
N201 Os2 C221 109.80(18) . .
C220 Os2 C221 37.78(18) . .
C216 Os2 C221 37.95(19) . .
N208 Os2 C217 115.85(16) . .
N201 Os2 C217 167.44(17) . .
C220 Os2 C217 80.0(2) . .
C216 Os2 C217 37.59(19) . .
C221 Os2 C217 68.4(2) . .
N208 Os2 C219 163.5(2) . .
N201 Os2 C219 100.80(17) . .
C220 Os2 C219 38.1(2) . .
C216 Os2 C219 79.70(18) . .
C221 Os2 C219 68.56(19) . .
C217 Os2 C219 66.79(19) . .
N208 Os2 C218 151.99(17) . .
N201 Os2 C218 130.58(17) . .
C220 Os2 C218 67.9(2) . .
C216 Os2 C218 67.85(19) . .
C221 Os2 C218 81.2(2) . .
C217 Os2 C218 37.44(18) . .
C219 Os2 C218 36.8(2) . .
N208 Os2 I2 85.06(12) . .
N201 Os2 I2 84.05(12) . .
C220 Os2 I2 147.29(14) . .
C216 Os2 I2 128.30(14) . .
C221 Os2 I2 166.09(13) . .
C217 Os2 I2 98.31(15) . .
C219 Os2 I2 111.03(15) . .
C218 Os2 I2 90.77(15) . .
C202 N201 C206 117.9(4) . .
C202 N201 Os2 125.9(3) . .
C206 N201 Os2 116.2(3) . .
N201 C202 C203 120.9(5) . .
N201 C202 H20A 119.5 . .
C203 C202 H20A 119.5 . .
C204 C203 C202 120.7(5) . .
C204 C203 H20B 119.7 . .
C202 C203 H20B 119.7 . .
C203 C204 C205 118.7(5) . .
C203 C204 H20C 120.6 . .
C205 C204 H20C 120.6 . .
C206 C205 C204 118.7(5) . .
C206 C205 H20D 120.7 . .
C204 C205 H20D 120.7 . .
N201 C206 C205 123.1(4) . .
N201 C206 C207 112.8(4) . .
C205 C206 C207 124.1(5) . .
N208 C207 C206 117.9(4) . .
N208 C207 H20E 121.1 . .
C206 C207 H20E 121.1 . .
C207 N208 C209 118.8(4) . .
C207 N208 Os2 116.5(3) . .
C209 N208 Os2 124.7(3) . .
C210 C209 C214 120.1(4) . .
C210 C209 N208 121.3(4) . .
C214 C209 N208 118.6(4) . .
C209 C210 C211 120.8(5) . .
C209 C210 H21A 119.6 . .
C211 C210 H21A 119.6 . .
C210 C211 C212 120.0(5) . .
C210 C211 H21B 120.0 . .
C212 C211 H21B 120.0 . .
C213 C212 O215 117.7(5) . .
C213 C212 C211 119.6(4) . .
O215 C212 C211 122.8(5) . .
C212 C213 C214 121.3(5) . .
C212 C213 H21C 119.4 . .
C214 C213 H21C 119.4 . .
C213 C214 C209 118.3(5) . .
C213 C214 H21D 120.9 . .
C209 C214 H21D 120.9 . .
C212 O215 H21H 109.5 . .
C217 C216 C221 121.6(5) . .
C217 C216 Os2 72.1(3) . .
C221 C216 Os2 71.7(3) . .
C217 C216 H21E 118.6 . .
C221 C216 H21E 118.6 . .
Os2 C216 H21E 118.6 . .
C216 C217 C218 120.7(5) . .
C216 C217 Os2 70.3(3) . .
C218 C217 Os2 72.7(3) . .
C216 C217 H21F 119.1 . .
C218 C217 H21F 119.1 . .
Os2 C217 H21F 119.1 . .
C219 C218 C217 118.2(5) . .
C219 C218 C225 120.7(5) . .
C217 C218 C225 121.0(5) . .
C219 C218 Os2 70.4(3) . .
C217 C218 Os2 69.9(3) . .
C225 C218 Os2 130.0(4) . .
C218 C219 C220 120.7(5) . .
C218 C219 Os2 72.9(3) . .
C220 C219 Os2 69.3(3) . .
C218 C219 H21G 118.9 . .
C220 C219 H21G 118.9 . .
Os2 C219 H21G 118.9 . .
C221 C220 C219 121.7(5) . .
C221 C220 Os2 72.4(3) . .
C219 C220 Os2 72.6(3) . .
C221 C220 H22K 118.7 . .
C219 C220 H22K 118.7 . .
Os2 C220 H22K 118.7 . .
C220 C221 C216 117.1(5) . .
C220 C221 C222 123.4(5) . .
C216 C221 C222 119.4(4) . .
C220 C221 Os2 69.9(3) . .
C216 C221 Os2 70.4(3) . .
C222 C221 Os2 127.5(3) . .
C223 C222 C221 113.0(4) . .
C223 C222 C224 110.9(5) . .
C221 C222 C224 109.9(4) . .
C223 C222 H22A 107.6 . .
C221 C222 H22A 107.6 . .
C224 C222 H22A 107.6 . .
C222 C223 H22B 109.5 . .
C222 C223 H22C 109.5 . .
H22B C223 H22C 109.5 . .
C222 C223 H22D 109.5 . .
H22B C223 H22D 109.5 . .
H22C C223 H22D 109.5 . .
C222 C224 H22E 109.5 . .
C222 C224 H22F 109.5 . .
H22E C224 H22F 109.5 . .
C222 C224 H22G 109.5 . .
H22E C224 H22G 109.5 . .
H22F C224 H22G 109.5 . .
C218 C225 H22H 109.5 . .
C218 C225 H22I 109.5 . .
H22H C225 H22I 109.5 . .
C218 C225 H22J 109.5 . .
H22H C225 H22J 109.5 . .
H22I C225 H22J 109.5 . .
F15 P10 F13 99.0(9) . .
F15 P10 F11 97.5(7) . .
F13 P10 F11 93.1(7) . .
F15 P10 F12A 102.4(6) . .
F13 P10 F12A 104.5(7) . .
F11 P10 F12A 150.8(7) . .
F15 P10 F16A 138.2(7) . .
F13 P10 F16A 112.4(7) . .
F11 P10 F16A 55.5(6) . .
F12A P10 F16A 95.8(6) . .
F15 P10 F12 80.8(8) . .
F13 P10 F12 99.7(8) . .
F11 P10 F12 167.3(8) . .
F12A P10 F12 23.3(7) . .
F16A P10 F12 118.1(8) . .
F15 P10 F14A 48.3(6) . .
F13 P10 F14A 144.2(7) . .
F11 P10 F14A 79.8(5) . .
F12A P10 F14A 97.9(5) . .
F16A P10 F14A 92.4(5) . .
F12 P10 F14A 89.9(7) . .
F15 P10 F13A 125.9(7) . .
F13 P10 F13A 29.5(6) . .
F11 P10 F13A 99.6(5) . .
F12A P10 F13A 85.8(5) . .
F16A P10 F13A 92.3(5) . .
F12 P10 F13A 91.5(7) . .
F14A P10 F13A 173.7(6) . .
F15 P10 F15A 40.0(5) . .
F13 P10 F15A 65.3(6) . .
F11 P10 F15A 118.7(6) . .
F12A P10 F15A 90.1(5) . .
F16A P10 F15A 174.1(5) . .
F12 P10 F15A 67.8(7) . .
F14A P10 F15A 87.3(4) . .
F13A P10 F15A 87.5(5) . .
F15 P10 F11A 79.5(6) . .
F13 P10 F11A 68.1(6) . .
F11 P10 F11A 33.8(5) . .
F12A P10 F11A 172.6(5) . .
F16A P10 F11A 87.2(5) . .
F12 P10 F11A 154.7(8) . .
F14A P10 F11A 88.8(4) . .
F13A P10 F11A 87.3(4) . .
F15A P10 F11A 86.9(5) . .
F15 P10 F16 170.1(7) . .
F13 P10 F16 90.6(7) . .
F11 P10 F16 84.3(6) . .
F12A P10 F16 72.5(6) . .
F16A P10 F16 36.9(4) . .
F12 P10 F16 95.2(8) . .
F14A P10 F16 123.0(6) . .
F13A P10 F16 63.0(5) . .
F15A P10 F16 146.2(5) . .
F11A P10 F16 106.6(5) . .
F15 P10 F14 88.1(7) . .
F13 P10 F14 172.7(7) . .
F11 P10 F14 87.6(6) . .
F12A P10 F14 72.2(5) . .
F16A P10 F14 62.2(5) . .
F12 P10 F14 79.8(7) . .
F14A P10 F14 43.0(4) . .
F13A P10 F14 143.3(6) . .
F15A P10 F14 120.5(4) . .
F11A P10 F14 115.2(5) . .
F16 P10 F14 82.2(6) . .
F22 P20 F22 180.0(3) 2_655 .
F22 P20 F21 90.1(2) 2_655 .
F22 P20 F21 89.9(2) . .
F22 P20 F21 89.9(2) 2_655 2_655
F22 P20 F21 90.1(2) . 2_655
F21 P20 F21 180.0(2) . 2_655
F22 P20 F23 89.92(17) 2_655 .
F22 P20 F23 90.08(17) . .
F21 P20 F23 89.93(17) . .
F21 P20 F23 90.07(17) 2_655 .
F22 P20 F23 90.08(17) 2_655 2_655
F22 P20 F23 89.92(17) . 2_655
F21 P20 F23 90.07(17) . 2_655
F21 P20 F23 89.93(17) 2_655 2_655
F23 P20 F23 180.0(3) . 2_655
F31 P30 F31 180.0(3) 2 .
F31 P30 F32 90.09(19) 2 2
F31 P30 F32 89.91(19) . 2
F31 P30 F32 89.91(19) 2 .
F31 P30 F32 90.09(19) . .
F32 P30 F32 180.0(3) 2 .
F31 P30 F33 90.6(2) 2 .
F31 P30 F33 89.4(2) . .
F32 P30 F33 89.9(2) 2 .
F32 P30 F33 90.1(2) . .
F31 P30 F33 89.4(2) 2 2
F31 P30 F33 90.6(2) . 2
F32 P30 F33 90.1(2) 2 2
F32 P30 F33 89.9(2) . 2
F33 P30 F33 180.0(3) . 2
H30A O300 H30B 127(9) . .
Cl1 C500 Cl2 111.7(3) . .
Cl1 C500 H50A 109.3 . .
Cl2 C500 H50A 109.3 . .
Cl1 C500 H50B 109.3 . .
Cl2 C500 H50B 109.3 . .
H50A C500 H50B 107.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Os1 N108 2.077(4) .
Os1 N101 2.087(4) .
Os1 C120 2.182(5) .
Os1 C116 2.189(5) .
Os1 C117 2.206(5) .
Os1 C121 2.209(5) .
Os1 C119 2.219(4) .
Os1 C118 2.256(4) .
Os1 I1 2.7091(4) .
N101 C102 1.348(6) .
N101 C106 1.373(6) .
C102 C103 1.380(6) .
C102 H10A 0.9500 .
C103 C104 1.386(7) .
C103 H10B 0.9500 .
C104 C105 1.366(7) .
C104 H10C 0.9500 .
C105 C106 1.386(7) .
C105 H10D 0.9500 .
C106 C107 1.443(6) .
C107 N108 1.293(6) .
C107 H10E 0.9500 .
N108 C109 1.428(6) .
C109 C114 1.384(7) .
C109 C110 1.397(7) .
C110 C111 1.369(7) .
C110 H11A 0.9500 .
C111 C112 1.375(8) .
C111 H11B 0.9500 .
C112 O115 1.367(6) .
C112 C113 1.413(7) .
C113 C114 1.399(6) .
C113 H11C 0.9500 .
C114 H11D 0.9500 .
O115 H11H 0.8400 .
C116 C117 1.391(7) .
C116 C121 1.431(7) .
C116 H11E 1.0000 .
C117 C118 1.427(7) .
C117 H11F 1.0000 .
C118 C119 1.396(7) .
C118 C125 1.495(7) .
C119 C120 1.435(7) .
C119 H11G 1.0000 .
C120 C121 1.424(6) .
C120 H12K 1.0000 .
C121 C122 1.521(7) .
C122 C124 1.514(8) .
C122 C123 1.530(7) .
C122 H12J 1.0000 .
C123 H12A 0.9800 .
C123 H12B 0.9800 .
C123 H12C 0.9800 .
C124 H12D 0.9800 .
C124 H12E 0.9800 .
C124 H12F 0.9800 .
C125 H12G 0.9800 .
C125 H12H 0.9800 .
C125 H12I 0.9800 .
Os2 N208 2.078(4) .
Os2 N201 2.080(4) .
Os2 C220 2.169(5) .
Os2 C216 2.184(5) .
Os2 C221 2.201(6) .
Os2 C217 2.209(5) .
Os2 C219 2.212(5) .
Os2 C218 2.245(5) .
Os2 I2 2.7247(4) .
N201 C202 1.348(6) .
N201 C206 1.371(6) .
C202 C203 1.394(7) .
C202 H20A 0.9500 .
C203 C204 1.377(8) .
C203 H20B 0.9500 .
C204 C205 1.384(7) .
C204 H20C 0.9500 .
C205 C206 1.375(7) .
C205 H20D 0.9500 .
C206 C207 1.437(6) .
C207 N208 1.295(6) .
C207 H20E 0.9500 .
N208 C209 1.441(6) .
C209 C210 1.372(7) .
C209 C214 1.416(6) .
C210 C211 1.380(7) .
C210 H21A 0.9500 .
C211 C212 1.398(7) .
C211 H21B 0.9500 .
C212 C213 1.372(8) .
C212 O215 1.375(6) .
C213 C214 1.398(7) .
C213 H21C 0.9500 .
C214 H21D 0.9500 .
O215 H21H 0.8400 .
C216 C217 1.415(7) .
C216 C221 1.426(7) .
C216 H21E 1.0000 .
C217 C218 1.430(7) .
C217 H21F 1.0000 .
C218 C219 1.405(8) .
C218 C225 1.489(8) .
C219 C220 1.432(8) .
C219 H21G 1.0000 .
C220 C221 1.415(7) .
C220 H22K 1.0000 .
C221 C222 1.523(7) .
C222 C223 1.518(8) .
C222 C224 1.540(7) .
C222 H22A 1.0000 .
C223 H22B 0.9800 .
C223 H22C 0.9800 .
C223 H22D 0.9800 .
C224 H22E 0.9800 .
C224 H22F 0.9800 .
C224 H22G 0.9800 .
C225 H22H 0.9800 .
C225 H22I 0.9800 .
C225 H22J 0.9800 .
P10 F15 1.488(12) .
P10 F13 1.491(13) .
P10 F11 1.536(10) .
P10 F12A 1.566(7) .
P10 F16A 1.572(8) .
P10 F12 1.574(15) .
P10 F14A 1.576(7) .
P10 F13A 1.590(7) .
P10 F15A 1.633(7) .
P10 F11A 1.635(7) .
P10 F16 1.682(12) .
P10 F14 1.712(9) .
P20 F22 1.592(3) 2_655
P20 F22 1.592(3) .
P20 F21 1.598(3) .
P20 F21 1.598(3) 2_655
P20 F23 1.598(3) .
P20 F23 1.598(3) 2_655
P30 F31 1.579(3) 2
P30 F31 1.579(3) .
P30 F32 1.583(3) 2
P30 F32 1.583(3) .
P30 F33 1.587(3) .
P30 F33 1.587(3) 2
O300 H30A 0.89(2) .
O300 H30B 0.89(2) .
C500 Cl1 1.727(6) .
C500 Cl2 1.825(7) .
C500 H50A 0.9900 .
C500 H50B 0.9900 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O115 H11H O400 0.84 1.84 2.671(6) 172.5 .
O215 H21H O300 0.84 1.89 2.727(7) 172.1 .
O300 H30A F33 0.89(2) 2.10(3) 2.984(7) 171(8) 1_655
O300 H30B F21 0.89(2) 2.36(3) 3.221(7) 164(8) 2_655
