#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:14:46 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179052 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/14/4301484.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_4301484
loop_
_publ_author_name
'Sabine H. van Rijt'
'Anna F. A. Peacock'
'Russell D. L. Johnstone'
'Simon Parsons'
'Peter J. Sadler'
_publ_contact_author_email       R.D.L.Johnstone@sms.ed.ac.uk
_publ_contact_author_name        R.D.L.Johnstone
_publ_section_title
;
Organometallic Osmium(II) Arene Anticancer Complexes Containing Picolinate
Derivatives
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1753
_journal_page_last               1762
_journal_paper_doi               10.1021/ic8020222
_journal_volume                  48
_journal_year                    2009
_chemical_compound_source        'S.Rijt reaction SVR05'
_chemical_formula_moiety         '[Os(C12H10)(C6H3O2NBr)(Cl)][CHCl3]'
_chemical_formula_sum            'C19 H14 Br Cl4 N O2 Os'
_chemical_formula_weight         700.22
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             06-11-27
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.783(7)
_cell_angle_beta                 98.387(8)
_cell_angle_gamma                91.757(7)
_cell_formula_units_Z            2
_cell_length_a                   6.8555(8)
_cell_length_b                   11.0638(11)
_cell_length_c                   13.9209(19)
_cell_measurement_reflns_used    1672
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.32
_cell_measurement_theta_min      2.60
_cell_volume                     1027.7(2)
_computing_cell_refinement       Saint
_computing_data_collection       Smart
_computing_data_reduction        Saint
_computing_molecular_graphics    Shelx-97
_computing_publication_material  Platon
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    Dirdif
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       sphere
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_sigmaI/netI    0.0807
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11370
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         28.47
_diffrn_reflns_theta_min         1.50
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    8.684
_exptl_absorpt_correction_T_max  0.300
_exptl_absorpt_correction_T_min  0.076
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    2.263
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             660
_exptl_crystal_recrystallization_method
;

Diffusion of diethyl ether into a solution of CHCl3 at ambient temperature in

;
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.917
_refine_diff_density_min         -2.286
_refine_diff_density_rms         0.263
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         4684
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0394P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0868
_reflns_number_gt                3601
_reflns_number_total             4684
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8020222_si_002_1.cif
_cod_data_source_block           1
_cod_database_code               4301484
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 0.05380(3) 0.21570(2) 0.202002(18) 0.02079(9) Uani 1 1 d . . .
Cl1 Cl -0.1852(2) 0.18671(15) 0.05401(12) 0.0277(4) Uani 1 1 d . . .
N1A N 0.0768(7) 0.3988(5) 0.1698(4) 0.0200(11) Uani 1 1 d . . .
C2A C 0.1944(9) 0.4473(6) 0.1155(5) 0.0240(14) Uani 1 1 d . . .
C3A C 0.1814(10) 0.5687(6) 0.0976(5) 0.0293(16) Uani 1 1 d . . .
H3A H 0.2700 0.6008 0.0605 0.035 Uiso 1 1 calc R . .
C4A C 0.0410(10) 0.6395(6) 0.1339(5) 0.0298(16) Uani 1 1 d . . .
H4A H 0.0304 0.7214 0.1223 0.036 Uiso 1 1 calc R . .
C5A C -0.0864(9) 0.5908(6) 0.1880(5) 0.0281(15) Uani 1 1 d . . .
H5A H -0.1866 0.6383 0.2134 0.034 Uiso 1 1 calc R . .
C6A C -0.0648(9) 0.4716(6) 0.2042(5) 0.0237(14) Uani 1 1 d . . .
Br2A Br 0.38510(10) 0.35274(6) 0.05965(5) 0.03373(18) Uani 1 1 d . . .
C61A C -0.2032(9) 0.4133(6) 0.2601(5) 0.0241(14) Uani 1 1 d . . .
O62A O -0.3338(7) 0.4701(4) 0.2946(3) 0.0312(11) Uani 1 1 d . . .
O63A O -0.1690(6) 0.3014(4) 0.2692(3) 0.0250(10) Uani 1 1 d . . .
C1B C 0.1357(9) 0.0270(6) 0.1632(5) 0.0282(15) Uani 1 1 d . . .
H1B H 0.0867 -0.0329 0.1067 0.034 Uiso 1 1 calc R . .
C2B C 0.3021(9) 0.1061(6) 0.1610(5) 0.0303(17) Uani 1 1 d . . .
H2B H 0.3677 0.0963 0.1048 0.036 Uiso 1 1 calc R . .
C3B C 0.3690(10) 0.1993(7) 0.2431(5) 0.0346(18) Uani 1 1 d . . .
H3B H 0.4763 0.2544 0.2404 0.042 Uiso 1 1 calc R . .
C4B C 0.2790(9) 0.2118(6) 0.3289(5) 0.0317(17) Uani 1 1 d . . .
H4B H 0.3281 0.2730 0.3845 0.038 Uiso 1 1 calc R . .
C5B C 0.1133(9) 0.1314(6) 0.3314(5) 0.0263(15) Uani 1 1 d . . .
H5B H 0.0504 0.1418 0.3885 0.032 Uiso 1 1 calc R . .
C6B C 0.0397(9) 0.0360(6) 0.2503(5) 0.0238(14) Uani 1 1 d . . .
C7B C -0.1367(9) -0.0429(6) 0.2529(5) 0.0233(14) Uani 1 1 d . . .
C8B C -0.1610(10) -0.0821(6) 0.3409(5) 0.0298(16) Uani 1 1 d . . .
H8B H -0.0623 -0.0603 0.3972 0.036 Uiso 1 1 calc R . .
C9B C -0.3279(10) -0.1525(7) 0.3464(5) 0.0358(18) Uani 1 1 d . . .
H9B H -0.3431 -0.1788 0.4065 0.043 Uiso 1 1 calc R . .
C10B C -0.4721(10) -0.1847(6) 0.2653(5) 0.0332(17) Uani 1 1 d . . .
H10B H -0.5885 -0.2308 0.2700 0.040 Uiso 1 1 calc R . .
C11B C -0.4466(10) -0.1494(6) 0.1768(5) 0.0308(16) Uani 1 1 d . . .
H11B H -0.5432 -0.1742 0.1199 0.037 Uiso 1 1 calc R . .
C12B C -0.2810(10) -0.0783(6) 0.1712(5) 0.0295(16) Uani 1 1 d . . .
H12B H -0.2656 -0.0534 0.1106 0.035 Uiso 1 1 calc R . .
C1S C -0.2340(10) 0.3368(6) 0.5033(5) 0.0318(16) Uani 1 1 d . . .
H1S H -0.2658 0.3671 0.4395 0.038 Uiso 1 1 calc R . .
Cl1S Cl -0.3003(3) 0.17747(18) 0.48341(14) 0.0403(4) Uani 1 1 d . . .
Cl2S Cl -0.3701(3) 0.41679(18) 0.58955(14) 0.0416(5) Uani 1 1 d . . .
Cl3S Cl 0.0211(3) 0.36132(18) 0.54478(14) 0.0410(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'
Br Br -0.2901 2.4595 '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'
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'
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
O63A Os1 N1A 77.35(18) . . ?
O63A Os1 C5B 85.8(2) . . ?
N1A Os1 C5B 136.3(2) . . ?
O63A Os1 C3B 135.9(2) . . ?
N1A Os1 C3B 96.1(2) . . ?
C5B Os1 C3B 68.9(2) . . ?
O63A Os1 C4B 101.3(2) . . ?
N1A Os1 C4B 105.9(2) . . ?
C5B Os1 C4B 38.5(2) . . ?
C3B Os1 C4B 37.8(3) . . ?
O63A Os1 C1B 135.7(2) . . ?
N1A Os1 C1B 145.1(2) . . ?
C5B Os1 C1B 69.0(3) . . ?
C3B Os1 C1B 68.5(3) . . ?
C4B Os1 C1B 81.5(3) . . ?
O63A Os1 C2B 167.02(19) . . ?
N1A Os1 C2B 112.3(2) . . ?
C5B Os1 C2B 81.2(2) . . ?
C3B Os1 C2B 37.6(3) . . ?
C4B Os1 C2B 68.2(3) . . ?
C1B Os1 C2B 37.9(2) . . ?
O63A Os1 C6B 100.4(2) . . ?
N1A Os1 C6B 174.4(2) . . ?
C5B Os1 C6B 38.2(2) . . ?
C3B Os1 C6B 81.9(2) . . ?
C4B Os1 C6B 69.4(2) . . ?
C1B Os1 C6B 38.7(2) . . ?
C2B Os1 C6B 69.2(2) . . ?
O63A Os1 Cl1 84.82(12) . . ?
N1A Os1 Cl1 81.74(13) . . ?
C5B Os1 Cl1 136.98(17) . . ?
C3B Os1 Cl1 138.1(2) . . ?
C4B Os1 Cl1 171.01(19) . . ?
C1B Os1 Cl1 89.56(18) . . ?
C2B Os1 Cl1 104.73(19) . . ?
C6B Os1 Cl1 103.25(16) . . ?
C2A N1A C6A 116.6(5) . . ?
C2A N1A Os1 130.4(4) . . ?
C6A N1A Os1 112.8(4) . . ?
N1A C2A C3A 122.6(6) . . ?
N1A C2A Br2A 120.0(5) . . ?
C3A C2A Br2A 117.4(5) . . ?
C4A C3A C2A 119.5(6) . . ?
C4A C3A H3A 120.2 . . ?
C2A C3A H3A 120.2 . . ?
C3A C4A C5A 119.2(6) . . ?
C3A C4A H4A 120.4 . . ?
C5A C4A H4A 120.4 . . ?
C6A C5A C4A 118.7(6) . . ?
C6A C5A H5A 120.7 . . ?
C4A C5A H5A 120.7 . . ?
N1A C6A C5A 123.4(6) . . ?
N1A C6A C61A 115.9(5) . . ?
C5A C6A C61A 120.7(6) . . ?
O62A C61A O63A 123.9(6) . . ?
O62A C61A C6A 121.4(6) . . ?
O63A C61A C6A 114.7(6) . . ?
C61A O63A Os1 119.1(4) . . ?
C2B C1B C6B 121.2(6) . . ?
C2B C1B Os1 72.1(4) . . ?
C6B C1B Os1 71.8(4) . . ?
C2B C1B H1B 119.4 . . ?
C6B C1B H1B 119.4 . . ?
Os1 C1B H1B 129.1 . . ?
C3B C2B C1B 119.5(6) . . ?
C3B C2B Os1 70.0(4) . . ?
C1B C2B Os1 70.0(4) . . ?
C3B C2B H2B 120.3 . . ?
C1B C2B H2B 120.3 . . ?
Os1 C2B H2B 132.8 . . ?
C4B C3B C2B 121.1(6) . . ?
C4B C3B Os1 71.2(4) . . ?
C2B C3B Os1 72.4(4) . . ?
C4B C3B H3B 119.5 . . ?
C2B C3B H3B 119.5 . . ?
Os1 C3B H3B 129.4 . . ?
C3B C4B C5B 119.3(7) . . ?
C3B C4B Os1 71.0(4) . . ?
C5B C4B Os1 70.1(3) . . ?
C3B C4B H4B 120.3 . . ?
C5B C4B H4B 120.3 . . ?
Os1 C4B H4B 131.4 . . ?
C6B C5B C4B 121.7(6) . . ?
C6B C5B Os1 72.8(3) . . ?
C4B C5B Os1 71.5(4) . . ?
C6B C5B H5B 119.1 . . ?
C4B C5B H5B 119.1 . . ?
Os1 C5B H5B 129.1 . . ?
C5B C6B C1B 117.1(6) . . ?
C5B C6B C7B 120.8(6) . . ?
C1B C6B C7B 121.9(6) . . ?
C5B C6B Os1 69.1(3) . . ?
C1B C6B Os1 69.6(3) . . ?
C7B C6B Os1 128.5(4) . . ?
C12B C7B C8B 118.6(6) . . ?
C12B C7B C6B 122.3(5) . . ?
C8B C7B C6B 119.1(6) . . ?
C9B C8B C7B 120.4(6) . . ?
C9B C8B H8B 119.8 . . ?
C7B C8B H8B 119.8 . . ?
C10B C9B C8B 120.4(6) . . ?
C10B C9B H9B 119.8 . . ?
C8B C9B H9B 119.8 . . ?
C9B C10B C11B 119.7(6) . . ?
C9B C10B H10B 120.2 . . ?
C11B C10B H10B 120.2 . . ?
C12B C11B C10B 120.0(6) . . ?
C12B C11B H11B 120.0 . . ?
C10B C11B H11B 120.0 . . ?
C11B C12B C7B 120.9(6) . . ?
C11B C12B H12B 119.6 . . ?
C7B C12B H12B 119.6 . . ?
Cl3S C1S Cl2S 111.0(4) . . ?
Cl3S C1S Cl1S 109.5(4) . . ?
Cl2S C1S Cl1S 109.9(4) . . ?
Cl3S C1S H1S 108.8 . . ?
Cl2S C1S H1S 108.8 . . ?
Cl1S C1S H1S 108.8 . . ?
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 O63A 2.077(4) . ?
Os1 N1A 2.154(5) . ?
Os1 C5B 2.159(6) . ?
Os1 C3B 2.175(6) . ?
Os1 C4B 2.177(6) . ?
Os1 C1B 2.178(7) . ?
Os1 C2B 2.207(7) . ?
Os1 C6B 2.208(6) . ?
Os1 Cl1 2.4065(15) . ?
N1A C2A 1.341(8) . ?
N1A C6A 1.369(8) . ?
C2A C3A 1.410(9) . ?
C2A Br2A 1.874(7) . ?
C3A C4A 1.359(9) . ?
C3A H3A 0.9500 . ?
C4A C5A 1.386(9) . ?
C4A H4A 0.9500 . ?
C5A C6A 1.384(8) . ?
C5A H5A 0.9500 . ?
C6A C61A 1.507(8) . ?
C61A O62A 1.219(8) . ?
C61A O63A 1.290(7) . ?
C1B C2B 1.424(9) . ?
C1B C6B 1.452(9) . ?
C1B H1B 0.9500 . ?
C2B C3B 1.413(10) . ?
C2B H2B 0.9500 . ?
C3B C4B 1.411(10) . ?
C3B H3B 0.9500 . ?
C4B C5B 1.429(9) . ?
C4B H4B 0.9500 . ?
C5B C6B 1.428(9) . ?
C5B H5B 0.9500 . ?
C6B C7B 1.478(8) . ?
C7B C12B 1.386(9) . ?
C7B C8B 1.396(8) . ?
C8B C9B 1.383(9) . ?
C8B H8B 0.9500 . ?
C9B C10B 1.376(9) . ?
C9B H9B 0.9500 . ?
C10B C11B 1.386(9) . ?
C10B H10B 0.9500 . ?
C11B C12B 1.381(9) . ?
C11B H11B 0.9500 . ?
C12B H12B 0.9500 . ?
C1S Cl3S 1.757(7) . ?
C1S Cl2S 1.764(7) . ?
C1S Cl1S 1.772(7) . ?
C1S H1S 1.0000 . ?
