#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:07:36 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180061 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/07/7050718.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_7050718
loop_
_publ_author_name
'Das, Chayan'
'Peng, Shie-Ming'
'Lee, Gene-Hsiang'
'Goswami, Sreebrata'
_publ_section_title
;
 Osmium(II) complexes of 2-[(arylamido)phenylazo]pyridines. New
 examples of deamination reactions---X-ray structure and redox
 propertiesElectronic supplementary information (ESI) available:
 partial energy level diagrams and molecular orbitals of 1a, 2a and 4a,
 UV-vis spectra of 4 complexes and cyclic voltammograms of 1b, 2b and
 4b. See http://www.rsc.org/suppdata/nj/b1/b108507g/
;
_journal_issue                   2
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              222
_journal_paper_doi               10.1039/b108507g
_journal_volume                  26
_journal_year                    2002
_chemical_formula_sum            'C28 H22 Br N7 Os'
_chemical_formula_weight         726.64
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 91.36(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.643(2)
_cell_length_b                   14.1915(18)
_cell_length_c                   13.850(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      12.00
_cell_measurement_theta_min      9.26
_cell_volume                     2680.8(8)
_computing_cell_refinement       'Enraf-Nonius CAD4'
_computing_data_collection       'Enraf-Nonius CAD4'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       'ω--2θ scans'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0526
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4731
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.278
_exptl_absorpt_correction_T_max  0.5687
_exptl_absorpt_correction_T_min  0.2181
_exptl_absorpt_correction_type   'empirical used psi-scan'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.800
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.938
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4731
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0353
_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)+(0.0281P)²+0.0000P] where  P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0650
_refine_ls_wR_factor_ref         0.0717
_reflns_number_gt                3025
_reflns_number_total             4731
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b108507g.txt
_cod_data_source_block           ic7676
_cod_depositor_comments
;
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_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7050718
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Os Os 0.007254(19) 0.293133(18) 0.71530(2) 0.05351(11) Uani 1 1 d . . .
Br Br -0.06032(6) 0.44792(5) 0.77569(6) 0.0808(3) Uani 1 1 d . . .
N1 N -0.0580(4) 0.3306(3) 0.5836(4) 0.0573(16) Uani 1 1 d . . .
N2 N 0.1064(4) 0.3768(4) 0.5569(4) 0.0562(15) Uani 1 1 d . . .
N3 N 0.1142(4) 0.3527(3) 0.6483(4) 0.0491(14) Uani 1 1 d . . .
N4 N 0.1057(4) 0.3018(3) 0.8241(4) 0.0617(16) Uani 1 1 d . . .
N5 N -0.1016(4) 0.2141(4) 0.7806(4) 0.0606(15) Uani 1 1 d . . .
N6 N -0.0295(4) 0.0928(3) 0.6936(4) 0.0582(15) Uani 1 1 d . . .
N7 N 0.0303(4) 0.1650(3) 0.6730(4) 0.0525(14) Uani 1 1 d . . .
C1 C -0.1513(6) 0.3289(5) 0.5515(7) 0.080(3) Uani 1 1 d . . .
H1A H -0.1995 0.3076 0.5926 0.096 Uiso 1 1 calc R . .
C2 C -0.1781(7) 0.3573(6) 0.4605(8) 0.089(3) Uani 1 1 d . . .
H2A H -0.2436 0.3546 0.4405 0.106 Uiso 1 1 calc R . .
C3 C -0.1082(6) 0.3901(5) 0.3979(7) 0.084(3) Uani 1 1 d . . .
H3A H -0.1256 0.4104 0.3360 0.100 Uiso 1 1 calc R . .
C4 C -0.0130(6) 0.3918(5) 0.4301(6) 0.072(2) Uani 1 1 d . . .
H4A H 0.0354 0.4117 0.3886 0.086 Uiso 1 1 calc R . .
C5 C 0.0132(5) 0.3645(4) 0.5237(5) 0.0548(18) Uani 1 1 d . . .
C6 C 0.1979(4) 0.3714(4) 0.7014(5) 0.0505(17) Uani 1 1 d . . .
C7 C 0.2818(5) 0.4118(4) 0.6636(6) 0.062(2) Uani 1 1 d . . .
H7A H 0.2836 0.4278 0.5986 0.074 Uiso 1 1 calc R . .
C8 C 0.3601(5) 0.4274(5) 0.7221(6) 0.069(2) Uani 1 1 d . . .
H8A H 0.4160 0.4554 0.6978 0.083 Uiso 1 1 calc R . .
C9 C 0.3575(5) 0.4021(5) 0.8180(6) 0.069(2) Uani 1 1 d . . .
H9A H 0.4128 0.4127 0.8572 0.082 Uiso 1 1 calc R . .
C10 C 0.2759(5) 0.3616(4) 0.8582(5) 0.064(2) Uani 1 1 d . . .
H10A H 0.2760 0.3454 0.9233 0.077 Uiso 1 1 calc R . .
C11 C 0.1931(5) 0.3454(4) 0.7992(6) 0.0557(18) Uani 1 1 d . . .
C12 C 0.0896(5) 0.2799(5) 0.9230(6) 0.065(2) Uani 1 1 d . . .
C13 C 0.0947(6) 0.3467(6) 0.9952(7) 0.097(3) Uani 1 1 d . . .
H13A H 0.1105 0.4088 0.9808 0.117 Uiso 1 1 calc R . .
C14 C 0.0760(8) 0.3205(7) 1.0900(7) 0.121(4) Uani 1 1 d . . .
H14A H 0.0796 0.3652 1.1390 0.145 Uiso 1 1 calc R . .
C15 C 0.0522(7) 0.2290(9) 1.1112(7) 0.118(4) Uani 1 1 d . . .
H15A H 0.0412 0.2114 1.1747 0.141 Uiso 1 1 calc R . .
C16 C 0.0448(6) 0.1642(6) 1.0392(7) 0.094(3) Uani 1 1 d . . .
H16A H 0.0262 0.1029 1.0536 0.112 Uiso 1 1 calc R . .
C17 C 0.0642(5) 0.1877(5) 0.9462(6) 0.075(2) Uani 1 1 d . . .
H17A H 0.0604 0.1421 0.8981 0.090 Uiso 1 1 calc R . .
C18 C -0.1677(5) 0.2412(6) 0.8460(6) 0.087(3) Uani 1 1 d . . .
H18A H -0.1687 0.3040 0.8652 0.104 Uiso 1 1 calc R . .
C19 C -0.2328(6) 0.1809(6) 0.8846(7) 0.092(3) Uani 1 1 d . . .
H19A H -0.2778 0.2026 0.9288 0.110 Uiso 1 1 calc R . .
C20 C -0.2322(6) 0.0875(6) 0.8585(6) 0.083(3) Uani 1 1 d . . .
H20A H -0.2763 0.0453 0.8849 0.099 Uiso 1 1 calc R . .
C21 C -0.1663(5) 0.0582(5) 0.7937(6) 0.072(2) Uani 1 1 d . . .
H21A H -0.1651 -0.0047 0.7751 0.086 Uiso 1 1 calc R . .
C22 C -0.1001(5) 0.1214(5) 0.7546(5) 0.0579(18) Uani 1 1 d . . .
C23 C 0.1086(5) 0.1368(4) 0.6122(5) 0.0480(16) Uani 1 1 d . . .
C24 C 0.0874(6) 0.1005(5) 0.5238(6) 0.082(2) Uani 1 1 d . . .
H24A H 0.0228 0.0959 0.5013 0.099 Uiso 1 1 calc R . .
C25 C 0.1638(9) 0.0703(6) 0.4674(7) 0.106(4) Uani 1 1 d . . .
H25A H 0.1503 0.0435 0.4073 0.127 Uiso 1 1 calc R . .
C26 C 0.2572(8) 0.0796(6) 0.4989(8) 0.110(4) Uani 1 1 d . . .
H26A H 0.3080 0.0606 0.4598 0.132 Uiso 1 1 calc R . .
C27 C 0.2778(6) 0.1162(6) 0.5871(8) 0.098(3) Uani 1 1 d . . .
H27A H 0.3426 0.1213 0.6087 0.118 Uiso 1 1 calc R . .
C28 C 0.2029(5) 0.1460(5) 0.6452(6) 0.069(2) Uani 1 1 d . . .
H28A H 0.2166 0.1719 0.7057 0.083 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
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
N7 Os N3 97.7(2) . . ?
N7 Os N4 100.1(2) . . ?
N3 Os N4 80.5(2) . . ?
N7 Os N1 92.5(2) . . ?
N3 Os N1 77.3(2) . . ?
N4 Os N1 155.7(2) . . ?
N7 Os N5 75.5(2) . . ?
N3 Os N5 173.2(2) . . ?
N4 Os N5 100.3(2) . . ?
N1 Os N5 102.9(2) . . ?
N7 Os Br 167.59(15) . . ?
N3 Os Br 93.67(14) . . ?
N4 Os Br 86.63(14) . . ?
N1 Os Br 85.19(13) . . ?
N5 Os Br 93.12(15) . . ?
C1 N1 C5 118.9(7) . . ?
C1 N1 Os 132.1(6) . . ?
C5 N1 Os 108.9(5) . . ?
N3 N2 C5 110.4(5) . . ?
N2 N3 C6 121.0(5) . . ?
N2 N3 Os 122.0(4) . . ?
C6 N3 Os 117.0(5) . . ?
C11 N4 C12 119.1(6) . . ?
C11 N4 Os 113.8(5) . . ?
C12 N4 Os 126.5(4) . . ?
C18 N5 C22 117.8(6) . . ?
C18 N5 Os 129.3(5) . . ?
C22 N5 Os 112.9(4) . . ?
N7 N6 C22 110.3(5) . . ?
N6 N7 C23 112.1(5) . . ?
N6 N7 Os 123.2(4) . . ?
C23 N7 Os 124.6(4) . . ?
N1 C1 C2 122.2(8) . . ?
C1 C2 C3 120.3(9) . . ?
C4 C3 C2 117.8(8) . . ?
C3 C4 C5 121.4(8) . . ?
N2 C5 N1 120.6(7) . . ?
N2 C5 C4 120.0(7) . . ?
N1 C5 C4 119.3(7) . . ?
N3 C6 C7 124.1(7) . . ?
N3 C6 C11 114.2(6) . . ?
C7 C6 C11 121.7(6) . . ?
C8 C7 C6 119.4(7) . . ?
C7 C8 C9 120.0(7) . . ?
C8 C9 C10 122.4(7) . . ?
C9 C10 C11 118.7(7) . . ?
N4 C11 C10 127.7(7) . . ?
N4 C11 C6 114.4(6) . . ?
C10 C11 C6 117.8(6) . . ?
C13 C12 C17 119.1(7) . . ?
C13 C12 N4 122.8(7) . . ?
C17 C12 N4 118.1(7) . . ?
C12 C13 C14 119.5(8) . . ?
C15 C14 C13 120.2(9) . . ?
C16 C15 C14 119.8(9) . . ?
C15 C16 C17 121.0(8) . . ?
C16 C17 C12 120.2(8) . . ?
N5 C18 C19 122.7(7) . . ?
C18 C19 C20 119.9(8) . . ?
C21 C20 C19 118.6(7) . . ?
C20 C21 C22 120.6(7) . . ?
N6 C22 N5 117.9(5) . . ?
N6 C22 C21 121.7(6) . . ?
N5 C22 C21 120.3(6) . . ?
C24 C23 C28 121.4(7) . . ?
C24 C23 N7 119.4(7) . . ?
C28 C23 N7 119.2(6) . . ?
C23 C24 C25 118.7(9) . . ?
C26 C25 C24 120.5(10) . . ?
C25 C26 C27 120.5(9) . . ?
C26 C27 C28 120.2(9) . . ?
C23 C28 C27 118.7(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
Os N7 1.938(5) . ?
Os N3 1.941(5) . ?
Os N4 1.998(6) . ?
Os N1 2.079(6) . ?
Os N5 2.084(5) . ?
Os Br 2.5321(8) . ?
N1 C1 1.340(9) . ?
N1 C5 1.378(8) . ?
N2 N3 1.313(7) . ?
N2 C5 1.353(7) . ?
N3 C6 1.369(7) . ?
N4 C11 1.395(8) . ?
N4 C12 1.426(9) . ?
N5 C18 1.349(8) . ?
N5 C22 1.364(8) . ?
N6 N7 1.345(6) . ?
N6 C22 1.359(7) . ?
N7 C23 1.433(7) . ?
C1 C2 1.364(11) . ?
C2 C3 1.385(11) . ?
C3 C4 1.363(9) . ?
C4 C5 1.392(9) . ?
C6 C7 1.394(8) . ?
C6 C11 1.406(9) . ?
C7 C8 1.343(9) . ?
C8 C9 1.378(9) . ?
C9 C10 1.383(9) . ?
C10 C11 1.398(9) . ?
C12 C13 1.379(10) . ?
C12 C17 1.393(9) . ?
C13 C14 1.393(11) . ?
C14 C15 1.372(12) . ?
C15 C16 1.358(12) . ?
C16 C17 1.362(10) . ?
C18 C19 1.353(9) . ?
C19 C20 1.374(10) . ?
C20 C21 1.351(9) . ?
C21 C22 1.392(8) . ?
C23 C24 1.354(9) . ?
C23 C28 1.360(9) . ?
C24 C25 1.385(11) . ?
C25 C26 1.344(13) . ?
C26 C27 1.350(12) . ?
C27 C28 1.383(10) . ?
