#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:42:34 +0100 (Wed 23 de Mar de 2016) $
#$Revision: 179343 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/40/4324079.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_4324079
loop_
_publ_author_name
'Debasish Saha'
'Shyamal Das'
'Dinesh Maity'
'Supriya Dutta'
'Sujoy Baitalik'
_publ_section_title
;
 Synthesis, Structural Characterization, and Photophysical,
 Electrochemical, Intercomponent Energy-Transfer, and Anion-Sensing
 Studies of Imidazole 4,5-Bis(benzimidazole)-Bridged OsIIOsII and RuIIOsII
 Bipyridine Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              46
_journal_page_last               61
_journal_paper_doi               10.1021/ic100905u
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C59 H47 Cl7 N14 O13 Os2'
_chemical_formula_weight         1788.66
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 91.886(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.5661(7)
_cell_length_b                   20.3194(12)
_cell_length_c                   12.8467(7)
_cell_measurement_reflns_used    9091
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.45
_cell_volume                     3278.4(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      120(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0388
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            45594
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.59
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    4.231
_exptl_absorpt_correction_T_max  0.4563
_exptl_absorpt_correction_T_min  0.2963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.812
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             1748
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_platon_squeeze_details
;
;
_refine_diff_density_max         3.553
_refine_diff_density_min         -1.369
_refine_diff_density_rms         0.326
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.242
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         7710
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.242
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0619
_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)+(0.1400P)²+9.5000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2125
_refine_ls_wR_factor_ref         0.2174
_reflns_number_gt                6711
_reflns_number_total             7710
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100905u_si_002.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 1 21/m 1 '
_cod_database_code               4324079
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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 0.78236(2) 0.099003(13) 0.75157(2) 0.02444(15) Uani 1 1 d . . .
C1 C 0.6764(4) 0.0582(3) 0.5250(4) 0.0084(10) Uani 1 1 d . . .
C2 C 0.6558(5) -0.0096(3) 0.5324(5) 0.0130(11) Uani 1 1 d . . .
H2 H 0.6705 -0.0334 0.5948 0.016 Uiso 1 1 calc R . .
C3 C 0.6131(5) -0.0397(3) 0.4441(5) 0.0169(12) Uani 1 1 d . . .
H3 H 0.5987 -0.0856 0.4457 0.020 Uiso 1 1 calc R . .
C4 C 0.5902(5) -0.0042(3) 0.3518(6) 0.0226(14) Uani 1 1 d . . .
H4 H 0.5606 -0.0269 0.2930 0.027 Uiso 1 1 calc R . .
C5 C 0.6095(6) 0.0621(3) 0.3442(5) 0.0204(13) Uani 1 1 d . . .
H5 H 0.5941 0.0858 0.2818 0.025 Uiso 1 1 calc R . .
C6 C 0.6531(5) 0.0931(3) 0.4333(5) 0.0122(11) Uani 1 1 d . . .
C7 C 0.7204(4) 0.1615(3) 0.5523(4) 0.0104(10) Uani 1 1 d . . .
C8 C 0.7584(4) 0.2152(2) 0.6134(4) 0.0090(10) Uani 1 1 d . . .
C9 C 0.8260(6) 0.2500 0.7649(6) 0.0109(15) Uiso 1 2 d S . .
H9 H 0.8567 0.2500 0.8335 0.013 Uiso 1 2 calc SR . .
C10 C 0.9398(5) 0.1185(4) 0.9340(6) 0.0236(14) Uani 1 1 d . . .
H10 H 0.9921 0.1035 0.8878 0.028 Uiso 1 1 calc R . .
C11 C 0.9723(7) 0.1396(5) 1.0318(7) 0.0363(18) Uani 1 1 d . . .
H11 H 1.0458 0.1398 1.0516 0.044 Uiso 1 1 calc R . .
C12 C 0.8958(8) 0.1609(5) 1.1024(6) 0.039(2) Uani 1 1 d . . .
H12 H 0.9160 0.1749 1.1707 0.047 Uiso 1 1 calc R . .
C13 C 0.7908(7) 0.1606(4) 1.0686(5) 0.0274(15) Uani 1 1 d . . .
H13 H 0.7373 0.1748 1.1141 0.033 Uiso 1 1 calc R . .
C14 C 0.7620(5) 0.1396(3) 0.9675(5) 0.0173(12) Uani 1 1 d . . .
C15 C 0.6532(5) 0.1440(3) 0.9219(5) 0.0144(11) Uani 1 1 d . . .
C16 C 0.5646(6) 0.1637(3) 0.9775(6) 0.0247(14) Uani 1 1 d . . .
H16 H 0.5711 0.1718 1.0503 0.030 Uiso 1 1 calc R . .
C17 C 0.4672(6) 0.1712(3) 0.9246(6) 0.0247(15) Uani 1 1 d . . .
H17 H 0.4059 0.1839 0.9610 0.030 Uiso 1 1 calc R . .
C18 C 0.4601(5) 0.1602(3) 0.8187(6) 0.0222(13) Uani 1 1 d . . .
H18 H 0.3949 0.1672 0.7809 0.027 Uiso 1 1 calc R . .
C19 C 0.5499(5) 0.1387(3) 0.7682(5) 0.0159(12) Uani 1 1 d . . .
H19 H 0.5442 0.1303 0.6954 0.019 Uiso 1 1 calc R . .
C20 C 0.6817(5) -0.0300(3) 0.8183(5) 0.0187(12) Uani 1 1 d . . .
H20 H 0.6258 -0.0033 0.8428 0.022 Uiso 1 1 calc R . .
C21 C 0.6725(7) -0.0968(3) 0.8275(6) 0.0264(16) Uani 1 1 d . . .
H21 H 0.6119 -0.1158 0.8581 0.032 Uiso 1 1 calc R . .
C22 C 0.7547(6) -0.1369(4) 0.7906(6) 0.0311(16) Uiso 1 1 d . . .
H22 H 0.7511 -0.1834 0.7970 0.037 Uiso 1 1 calc R . .
C23 C 0.8403(6) -0.1075(4) 0.7452(6) 0.0253(15) Uiso 1 1 d . . .
H23 H 0.8955 -0.1337 0.7179 0.030 Uiso 1 1 calc R . .
C24 C 0.8454(5) -0.0388(3) 0.7397(5) 0.0167(12) Uiso 1 1 d . . .
C25 C 0.9344(5) -0.0025(3) 0.6943(5) 0.0157(12) Uani 1 1 d . . .
C26 C 1.0233(6) -0.0322(4) 0.6541(6) 0.0282(16) Uani 1 1 d . . .
H26 H 1.0299 -0.0788 0.6534 0.034 Uiso 1 1 calc R . .
C27 C 1.1034(6) 0.0078(5) 0.6146(7) 0.0374(19) Uani 1 1 d . . .
H27 H 1.1651 -0.0114 0.5864 0.045 Uiso 1 1 calc R . .
C28 C 1.0919(6) 0.0749(5) 0.6170(7) 0.0358(19) Uani 1 1 d . . .
H28 H 1.1466 0.1025 0.5924 0.043 Uiso 1 1 calc R . .
C29 C 1.0001(6) 0.1022(3) 0.6554(6) 0.0236(15) Uani 1 1 d . . .
H29 H 0.9915 0.1486 0.6544 0.028 Uiso 1 1 calc R . .
C30 C 0.7332(9) 0.9574(6) 0.1206(9) 0.057(3) Uani 1 1 d . . .
H30A H 0.7408 0.9610 0.1974 0.068 Uiso 1 1 calc R . .
H30B H 0.7247 0.9102 0.1031 0.068 Uiso 1 1 calc R . .
Cl1 Cl 0.1708(2) 0.2500 0.8462(4) 0.0515(9) Uani 1 2 d S . .
Cl2 Cl 0.5046(2) 0.2500 0.2634(2) 0.0332(6) Uani 1 2 d S . .
Cl3 Cl 0.0536(2) 0.7500 0.61458(18) 0.0252(5) Uani 1 2 d S . .
Cl4 Cl 0.61631(16) 1.00048(10) 0.07767(15) 0.0341(4) Uani 1 1 d . . .
Cl5 Cl 0.8465(2) 0.98594(14) 0.0669(3) 0.0612(8) Uani 1 1 d . . .
N1 N 0.7195(4) 0.1019(2) 0.5989(4) 0.0076(9) Uani 1 1 d . . .
N2 N 0.6809(4) 0.1580(2) 0.4530(4) 0.0126(10) Uani 1 1 d . . .
H2A H 0.6742 0.1910 0.4089 0.015 Uiso 1 1 calc R . .
N3 N 0.8011(4) 0.1953(2) 0.7092(4) 0.0085(9) Uani 1 1 d . . .
N4 N 0.8349(4) 0.1183(3) 0.9005(4) 0.0145(10) Uani 1 1 d . . .
N5 N 0.6454(4) 0.1293(2) 0.8187(4) 0.0130(10) Uani 1 1 d . . .
N6 N 0.7649(4) -0.0003(2) 0.7770(4) 0.0128(9) Uani 1 1 d . . .
N7 N 0.9221(4) 0.0640(3) 0.6946(4) 0.0136(10) Uani 1 1 d . . .
O1 O 0.0598(7) 0.2500 0.8335(13) 0.085(4) Uani 1 2 d S . .
O2 O 0.1998(18) 0.2014(11) 0.9091(16) 0.178(8) Uiso 1 1 d . . .
O3 O 0.227(4) 0.2500 0.762(3) 0.25(2) Uiso 1 2 d S . .
O4 O 0.4658(7) 0.1941(3) 0.3228(6) 0.0542(18) Uani 1 1 d . . .
O5 O 0.6178(9) 0.2500 0.2721(10) 0.062(3) Uani 1 2 d S . .
O6 O 0.4536(7) 0.2500 0.1616(6) 0.0330(17) Uani 1 2 d S . .
O7 O -0.0157(7) 0.7500 0.6999(6) 0.0352(19) Uani 1 2 d S . .
O8 O 0.1636(8) 0.7500 0.6567(8) 0.045(2) Uani 1 2 d S . .
O9 O 0.0392(7) 0.8081(3) 0.5551(6) 0.055(2) Uani 1 1 d . . .
O10 O 0.4498(6) 0.2500 0.5764(5) 0.0305(17) Uani 1 2 d S . .
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'
Cl Cl 0.1484 0.1585 '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 Os1 N5 78.3(2) . . ?
N4 Os1 N3 91.7(2) . . ?
N5 Os1 N3 86.00(18) . . ?
N4 Os1 N7 98.4(2) . . ?
N5 Os1 N7 175.4(2) . . ?
N3 Os1 N7 97.46(19) . . ?
N4 Os1 N6 94.1(2) . . ?
N5 Os1 N6 97.6(2) . . ?
N3 Os1 N6 173.67(19) . . ?
N7 Os1 N6 79.2(2) . . ?
N4 Os1 N1 167.0(2) . . ?
N5 Os1 N1 95.2(2) . . ?
N3 Os1 N1 76.50(18) . . ?
N7 Os1 N1 88.7(2) . . ?
N6 Os1 N1 97.93(18) . . ?
N1 C1 C6 108.5(5) . . ?
N1 C1 C2 130.3(5) . . ?
C6 C1 C2 121.3(5) . . ?
C3 C2 C1 116.6(6) . . ?
C2 C3 C4 121.8(6) . . ?
C5 C4 C3 122.0(6) . . ?
C4 C5 C6 116.6(6) . . ?
N2 C6 C1 106.5(5) . . ?
N2 C6 C5 131.7(6) . . ?
C1 C6 C5 121.8(5) . . ?
N1 C7 N2 111.3(5) . . ?
N1 C7 C8 116.9(5) . . ?
N2 C7 C8 131.8(5) . . ?
N3 C8 C8 107.0(3) . 4_565 ?
N3 C8 C7 112.3(5) . . ?
C8 C8 C7 140.4(3) 4_565 . ?
N3 C9 N3 110.5(7) 4_565 . ?
N4 C10 C11 122.7(7) . . ?
C10 C11 C12 119.6(7) . . ?
C13 C12 C11 117.6(7) . . ?
C12 C13 C14 120.6(7) . . ?
N4 C14 C13 121.9(6) . . ?
N4 C14 C15 114.0(5) . . ?
C13 C14 C15 123.8(6) . . ?
N5 C15 C16 121.9(6) . . ?
N5 C15 C14 114.2(5) . . ?
C16 C15 C14 123.9(6) . . ?
C17 C16 C15 118.9(6) . . ?
C18 C17 C16 119.5(6) . . ?
C17 C18 C19 119.0(6) . . ?
N5 C19 C18 122.6(6) . . ?
N6 C20 C21 123.6(7) . . ?
C20 C21 C22 118.6(7) . . ?
C23 C22 C21 118.9(7) . . ?
C22 C23 C24 119.5(7) . . ?
N6 C24 C23 120.9(6) . . ?
N6 C24 C25 115.4(5) . . ?
C23 C24 C25 123.7(6) . . ?
N7 C25 C26 121.8(6) . . ?
N7 C25 C24 114.1(5) . . ?
C26 C25 C24 124.2(6) . . ?
C25 C26 C27 118.8(7) . . ?
C28 C27 C26 119.3(7) . . ?
C27 C28 C29 119.8(7) . . ?
N7 C29 C28 121.4(6) . . ?
Cl5 C30 Cl4 113.5(6) . . ?
O3 Cl1 O2 111.0(15) . 4_565 ?
O3 Cl1 O2 111.0(15) . . ?
O2 Cl1 O2 96.9(19) 4_565 . ?
O3 Cl1 O1 118(2) . . ?
O2 Cl1 O1 109.0(11) 4_565 . ?
O2 Cl1 O1 109.0(11) . . ?
O5 Cl2 O6 119.0(7) . . ?
O5 Cl2 O4 108.0(5) . 4_565 ?
O6 Cl2 O4 109.2(4) . 4_565 ?
O5 Cl2 O4 108.0(5) . . ?
O6 Cl2 O4 109.2(4) . . ?
O4 Cl2 O4 102.1(7) 4_565 . ?
O9 Cl3 O9 113.1(7) 4_575 . ?
O9 Cl3 O7 110.3(4) 4_575 . ?
O9 Cl3 O7 110.3(4) . . ?
O9 Cl3 O8 107.5(4) 4_575 . ?
O9 Cl3 O8 107.5(4) . . ?
O7 Cl3 O8 108.0(6) . . ?
C7 N1 C1 106.1(5) . . ?
C7 N1 Os1 115.7(4) . . ?
C1 N1 Os1 138.2(4) . . ?
C7 N2 C6 107.6(5) . . ?
C9 N3 C8 107.8(5) . . ?
C9 N3 Os1 132.2(4) . . ?
C8 N3 Os1 118.1(3) . . ?
C14 N4 C10 117.6(6) . . ?
C14 N4 Os1 117.0(4) . . ?
C10 N4 Os1 124.9(5) . . ?
C15 N5 C19 117.9(5) . . ?
C15 N5 Os1 116.3(4) . . ?
C19 N5 Os1 125.6(4) . . ?
C20 N6 C24 118.5(5) . . ?
C20 N6 Os1 126.6(4) . . ?
C24 N6 Os1 114.7(4) . . ?
C29 N7 C25 118.9(5) . . ?
C29 N7 Os1 124.7(4) . . ?
C25 N7 Os1 116.3(4) . . ?
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 N4 2.041(5) . ?
Os1 N5 2.045(5) . ?
Os1 N3 2.047(4) . ?
Os1 N7 2.052(5) . ?
Os1 N6 2.058(5) . ?
Os1 N1 2.091(5) . ?
C1 N1 1.396(7) . ?
C1 C6 1.397(8) . ?
C1 C2 1.405(8) . ?
C2 C3 1.382(8) . ?
C3 C4 1.410(10) . ?
C4 C5 1.373(9) . ?
C5 C6 1.402(9) . ?
C6 N2 1.386(7) . ?
C7 N1 1.350(7) . ?
C7 N2 1.356(8) . ?
C7 C8 1.418(7) . ?
C8 N3 1.387(7) . ?
C8 C8 1.412(10) 4_565 ?
C9 N3 1.353(6) 4_565 ?
C9 N3 1.353(6) . ?
C10 N4 1.373(8) . ?
C10 C11 1.377(11) . ?
C11 C12 1.412(13) . ?
C12 C13 1.375(12) . ?
C13 C14 1.403(9) . ?
C14 N4 1.349(8) . ?
C14 C15 1.473(9) . ?
C15 N5 1.360(8) . ?
C15 C16 1.400(8) . ?
C16 C17 1.390(11) . ?
C17 C18 1.378(11) . ?
C18 C19 1.391(8) . ?
C19 N5 1.360(8) . ?
C20 N6 1.332(8) . ?
C20 C21 1.369(9) . ?
C21 C22 1.410(11) . ?
C22 C23 1.377(11) . ?
C23 C24 1.401(10) . ?
C24 N6 1.376(8) . ?
C24 C25 1.475(8) . ?
C25 N7 1.360(8) . ?
C25 C26 1.384(8) . ?
C26 C27 1.402(12) . ?
C27 C28 1.372(13) . ?
C28 C29 1.385(10) . ?
C29 N7 1.360(8) . ?
C30 Cl5 1.704(11) . ?
C30 Cl4 1.782(10) . ?
Cl1 O3 1.31(4) . ?
Cl1 O2 1.32(2) 4_565 ?
Cl1 O2 1.32(2) . ?
Cl1 O1 1.399(9) . ?
Cl2 O5 1.423(12) . ?
Cl2 O6 1.438(8) . ?
Cl2 O4 1.460(7) 4_565 ?
Cl2 O4 1.460(7) . ?
Cl3 O9 1.414(6) 4_575 ?
Cl3 O9 1.414(6) . ?
Cl3 O7 1.422(8) . ?
Cl3 O8 1.468(11) . ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.123 0.250 0.090 9 -1 ' '
2 0.227 0.250 0.474 67 11 ' '
3 0.772 0.750 0.526 67 14 ' '
4 0.877 0.750 0.910 9 -2 ' '
