#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:55:46 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179269 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/89/4318921.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_4318921
loop_
_publ_author_name
'Amit K. Ghosh'
'Kunal K. Kamar'
'Parimal Paul'
'Shie-Ming Peng'
'Gene-Hsiang Lee'
'Sreebrata Goswami'
_publ_section_title
;
 Photoinduced and Chemical Oxidation of Coordinated Imine to Amide in
 Isomeric Osmium(II) Complexes of N-Arylpyridine-2-carboxaldimines.
 Synthesis, Characterization, Electron Transfer Properties, and Structural
 Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6343
_journal_page_last               6350
_journal_paper_doi               10.1021/ic020454s
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C26 H24 Br2 N4 O2 Os'
_chemical_formula_weight         774.51
_chemical_name_systematic
;
 ?
;
_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                 94.53(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8976(12)
_cell_length_b                   18.370(4)
_cell_length_c                   15.956(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      11.34
_cell_measurement_theta_min      8.90
_cell_volume                     2599.8(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    0.0537
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4581
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.69
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    8.009
_exptl_absorpt_correction_T_max  0.5565
_exptl_absorpt_correction_T_min  0.1284
_exptl_absorpt_correction_type   'empirical used psi-scan'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.979
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.694
_refine_diff_density_min         -1.533
_refine_diff_density_rms         0.168
_refine_ls_extinction_coef       0.00046(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         4581
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0624P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1018
_refine_ls_wR_factor_ref         0.1146
_reflns_number_gt                2930
_reflns_number_total             4581
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020454s_1.cif
_cod_data_source_block           ic7674
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

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

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_cell_volume        2600.0(8)
_cod_database_code               4318921
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Os Os 0.03507(4) 0.35574(2) 0.74952(2) 0.04230(15) Uani 1 1 d . . .
Br1 Br -0.14496(17) 0.25061(7) 0.71921(7) 0.0895(5) Uani 1 1 d . . .
Br2 Br 0.25221(15) 0.26842(7) 0.78848(7) 0.0840(4) Uani 1 1 d . . .
O1 O -0.5057(8) 0.5712(4) 0.9109(5) 0.072(2) Uani 1 1 d . . .
O2 O 0.4724(8) 0.6020(5) 0.5583(5) 0.079(2) Uani 1 1 d . . .
N1 N 0.0611(9) 0.3566(4) 0.6226(4) 0.0485(19) Uani 1 1 d . . .
N2 N -0.1251(8) 0.4262(4) 0.7063(4) 0.049(2) Uani 1 1 d . . .
N3 N 0.0076(8) 0.3618(4) 0.8761(4) 0.0441(18) Uani 1 1 d . . .
N4 N 0.1710(7) 0.4388(4) 0.7856(4) 0.0389(17) Uani 1 1 d . . .
C1 C 0.1552(12) 0.3152(6) 0.5813(6) 0.063(3) Uani 1 1 d . . .
H1A H 0.2221 0.2846 0.6120 0.075 Uiso 1 1 calc R . .
C2 C 0.1562(13) 0.3167(7) 0.4950(6) 0.068(3) Uani 1 1 d . . .
H2A H 0.2223 0.2867 0.4688 0.082 Uiso 1 1 calc R . .
C3 C 0.0613(15) 0.3616(8) 0.4474(7) 0.082(4) Uani 1 1 d . . .
H3A H 0.0622 0.3632 0.3892 0.099 Uiso 1 1 calc R . .
C4 C -0.0365(13) 0.4048(7) 0.4895(6) 0.075(4) Uani 1 1 d . . .
H4A H -0.1019 0.4365 0.4593 0.089 Uiso 1 1 calc R . .
C5 C -0.0372(11) 0.4010(6) 0.5763(6) 0.052(3) Uani 1 1 d . . .
C6 C -0.1379(10) 0.4385(6) 0.6248(5) 0.058(3) Uani 1 1 d . . .
H6A H -0.2098 0.4704 0.6004 0.070 Uiso 1 1 calc R . .
C7 C -0.2226(10) 0.4650(5) 0.7581(5) 0.045(2) Uani 1 1 d . . .
C8 C -0.2297(11) 0.5402(6) 0.7562(6) 0.059(3) Uani 1 1 d . . .
H8A H -0.1695 0.5655 0.7212 0.071 Uiso 1 1 calc R . .
C9 C -0.3236(11) 0.5785(6) 0.8050(7) 0.062(3) Uani 1 1 d . . .
H9A H -0.3277 0.6291 0.8030 0.075 Uiso 1 1 calc R . .
C10 C -0.4114(9) 0.5397(6) 0.8569(6) 0.051(2) Uani 1 1 d . . .
C11 C -0.4061(10) 0.4644(6) 0.8600(7) 0.060(3) Uani 1 1 d . . .
H11A H -0.4661 0.4390 0.8951 0.072 Uiso 1 1 calc R . .
C12 C -0.3114(10) 0.4274(6) 0.8105(6) 0.053(3) Uani 1 1 d . . .
H12A H -0.3072 0.3768 0.8125 0.064 Uiso 1 1 calc R . .
C13 C -0.5094(14) 0.6489(8) 0.9143(10) 0.104(5) Uani 1 1 d . . .
H13A H -0.5808 0.6641 0.9529 0.157 Uiso 1 1 calc R . .
H13B H -0.5387 0.6679 0.8594 0.157 Uiso 1 1 calc R . .
H13C H -0.4111 0.6669 0.9330 0.157 Uiso 1 1 calc R . .
C14 C -0.0807(12) 0.3187(6) 0.9205(6) 0.060(3) Uani 1 1 d . . .
H14A H -0.1406 0.2835 0.8924 0.072 Uiso 1 1 calc R . .
C15 C -0.0838(12) 0.3255(6) 1.0056(6) 0.061(3) Uani 1 1 d . . .
H15A H -0.1473 0.2959 1.0343 0.073 Uiso 1 1 calc R . .
C16 C 0.0065(12) 0.3760(7) 1.0494(6) 0.066(3) Uani 1 1 d . . .
H16A H 0.0071 0.3794 1.1075 0.079 Uiso 1 1 calc R . .
C17 C 0.0964(11) 0.4215(6) 1.0053(6) 0.062(3) Uani 1 1 d . . .
H17A H 0.1569 0.4567 1.0328 0.074 Uiso 1 1 calc R . .
C18 C 0.0932(10) 0.4127(5) 0.9185(5) 0.047(2) Uani 1 1 d . . .
C19 C 0.1823(10) 0.4553(5) 0.8663(5) 0.048(2) Uani 1 1 d . . .
H19A H 0.2446 0.4926 0.8880 0.058 Uiso 1 1 calc R . .
C20 C 0.2514(9) 0.4830(5) 0.7303(5) 0.036(2) Uani 1 1 d . . .
C21 C 0.3440(9) 0.4499(5) 0.6757(6) 0.047(2) Uani 1 1 d . . .
H21A H 0.3563 0.3996 0.6766 0.057 Uiso 1 1 calc R . .
C22 C 0.4174(10) 0.4916(6) 0.6206(6) 0.053(3) Uani 1 1 d . . .
H22A H 0.4800 0.4695 0.5841 0.063 Uiso 1 1 calc R . .
C23 C 0.3992(10) 0.5647(6) 0.6189(6) 0.049(2) Uani 1 1 d . . .
C24 C 0.3117(10) 0.5994(6) 0.6749(6) 0.053(3) Uani 1 1 d . . .
H24A H 0.3034 0.6498 0.6751 0.064 Uiso 1 1 calc R . .
C25 C 0.2370(10) 0.5574(5) 0.7306(5) 0.047(2) Uani 1 1 d . . .
H25A H 0.1769 0.5797 0.7683 0.057 Uiso 1 1 calc R . .
C26 C 0.4393(15) 0.6789(8) 0.5455(9) 0.103(5) Uani 1 1 d . . .
H26A H 0.4943 0.6971 0.5005 0.154 Uiso 1 1 calc R . .
H26B H 0.4685 0.7053 0.5962 0.154 Uiso 1 1 calc R . .
H26C H 0.3332 0.6851 0.5314 0.154 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'
O O 0.0106 0.0060 '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
N4 Os N2 90.2(3) . . ?
N4 Os N3 78.0(3) . . ?
N2 Os N3 99.6(3) . . ?
N4 Os N1 99.5(3) . . ?
N2 Os N1 77.8(3) . . ?
N3 Os N1 176.5(3) . . ?
N4 Os Br1 174.11(19) . . ?
N2 Os Br1 90.3(2) . . ?
N3 Os Br1 96.1(2) . . ?
N1 Os Br1 86.4(2) . . ?
N4 Os Br2 88.88(19) . . ?
N2 Os Br2 173.4(2) . . ?
N3 Os Br2 86.62(19) . . ?
N1 Os Br2 95.9(2) . . ?
Br1 Os Br2 91.28(6) . . ?
C10 O1 C13 117.5(9) . . ?
C23 O2 C26 118.4(8) . . ?
C1 N1 C5 118.0(8) . . ?
C1 N1 Os 127.1(7) . . ?
C5 N1 Os 114.8(6) . . ?
C6 N2 C7 118.3(8) . . ?
C6 N2 Os 117.0(7) . . ?
C7 N2 Os 124.7(6) . . ?
C18 N3 C14 118.0(8) . . ?
C18 N3 Os 115.0(6) . . ?
C14 N3 Os 127.0(7) . . ?
C19 N4 C20 117.9(7) . . ?
C19 N4 Os 117.0(6) . . ?
C20 N4 Os 125.1(5) . . ?
N1 C1 C2 122.2(11) . . ?
C3 C2 C1 121.0(11) . . ?
C2 C3 C4 117.3(10) . . ?
C5 C4 C3 120.4(12) . . ?
N1 C5 C4 121.1(10) . . ?
N1 C5 C6 113.7(8) . . ?
C4 C5 C6 125.2(10) . . ?
N2 C6 C5 116.7(9) . . ?
C12 C7 C8 119.1(9) . . ?
C12 C7 N2 120.0(9) . . ?
C8 C7 N2 120.9(8) . . ?
C9 C8 C7 121.8(9) . . ?
C8 C9 C10 118.1(10) . . ?
O1 C10 C9 124.0(10) . . ?
O1 C10 C11 114.7(9) . . ?
C9 C10 C11 121.2(9) . . ?
C12 C11 C10 119.6(9) . . ?
C11 C12 C7 120.2(10) . . ?
N3 C14 C15 121.6(10) . . ?
C14 C15 C16 120.5(10) . . ?
C15 C16 C17 119.0(9) . . ?
C16 C17 C18 117.9(10) . . ?
N3 C18 C17 122.9(9) . . ?
N3 C18 C19 113.9(8) . . ?
C17 C18 C19 123.2(9) . . ?
N4 C19 C18 116.1(8) . . ?
C25 C20 C21 120.0(8) . . ?
C25 C20 N4 120.7(7) . . ?
C21 C20 N4 119.2(8) . . ?
C22 C21 C20 119.6(9) . . ?
C23 C22 C21 120.4(9) . . ?
C22 C23 C24 121.0(9) . . ?
C22 C23 O2 116.2(8) . . ?
C24 C23 O2 122.8(9) . . ?
C23 C24 C25 118.7(9) . . ?
C20 C25 C24 120.1(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 N4 2.003(7) . ?
Os N2 2.006(8) . ?
Os N3 2.056(7) . ?
Os N1 2.057(7) . ?
Os Br1 2.5313(12) . ?
Os Br2 2.5501(12) . ?
O1 C10 1.377(11) . ?
O1 C13 1.428(15) . ?
O2 C23 1.388(11) . ?
O2 C26 1.454(15) . ?
N1 C1 1.341(12) . ?
N1 C5 1.369(12) . ?
N2 C6 1.317(10) . ?
N2 C7 1.434(11) . ?
N3 C18 1.354(12) . ?
N3 C14 1.354(12) . ?
N4 C19 1.320(10) . ?
N4 C20 1.432(10) . ?
C1 C2 1.378(13) . ?
C2 C3 1.368(16) . ?
C3 C4 1.390(17) . ?
C4 C5 1.387(13) . ?
C5 C6 1.410(13) . ?
C7 C12 1.381(12) . ?
C7 C8 1.382(14) . ?
C8 C9 1.380(14) . ?
C9 C10 1.381(13) . ?
C10 C11 1.385(14) . ?
C11 C12 1.379(13) . ?
C14 C15 1.367(13) . ?
C15 C16 1.380(15) . ?
C16 C17 1.386(14) . ?
C17 C18 1.392(12) . ?
C18 C19 1.427(12) . ?
C20 C25 1.372(12) . ?
C20 C21 1.386(11) . ?
C21 C22 1.371(12) . ?
C22 C23 1.353(14) . ?
C23 C24 1.386(12) . ?
C24 C25 1.386(12) . ?
