#------------------------------------------------------------------------------
#$Date: 2016-03-26 21:37:51 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180479 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/48/7214891.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_7214891
loop_
_publ_author_name
'Xu, Feng'
'Peng, Yu-Xin'
'Hu, Bin'
'Tao, Tao'
'Huang, Wei'
_publ_section_title
;
 Comparative structural and spectral analyses for mononuclear and
 dinuclear metal complexes of 2-thiophen and 2-(5-bromothiophen)
 imidazo[4,5-f][1,10]phenanthroline
;
_journal_issue                   23
_journal_name_full               CrystEngComm
_journal_page_first              8023
_journal_paper_doi               10.1039/c2ce26001h
_journal_volume                  14
_journal_year                    2012
_chemical_formula_moiety         'C36 H26 Br2 Cl4 N8 Ni2 O2 S2'
_chemical_formula_sum            'C36 H26 Br2 Cl4 N8 Ni2 O2 S2'
_chemical_formula_weight         1085.81
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_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                109.506(2)
_cell_angle_beta                 93.424(2)
_cell_angle_gamma                102.044(2)
_cell_formula_units_Z            1
_cell_length_a                   8.1860(14)
_cell_length_b                   10.3316(17)
_cell_length_c                   12.858(2)
_cell_measurement_reflns_used    1630
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      27.736
_cell_measurement_theta_min      2.874
_cell_volume                     992.6(3)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker 2000)'
_computing_data_reduction        'SAINT (Bruker 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXTL (BRUKER 2000)'
_computing_structure_solution    'SHELXTL (BRUKER 2000)'
_diffrn_ambient_temperature      291(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker Smart Apex CCD area detector'
_diffrn_measurement_method       'φ and ω 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  0.0468
_diffrn_reflns_av_sigmaI/netI    0.0704
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4998
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.70
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.382
_exptl_absorpt_correction_T_max  0.7285
_exptl_absorpt_correction_T_min  0.6870
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker(2000)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.817
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.663
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.910
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3434
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.910
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0387
_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)+(0.0452P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.0991
_reflns_number_gt                2371
_reflns_number_total             3434
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce26001h.txt
_cod_data_source_block           7
_cod_database_code               7214891
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
Ni1 Ni 0.40457(7) 0.37852(5) 0.55431(5) 0.03185(18) Uani 1 1 d .
Br1 Br -0.17507(9) -0.43493(6) 1.07956(5) 0.0689(2) Uani 1 1 d .
C1 C 0.6076(6) 0.3074(5) 0.7271(4) 0.0383(11) Uani 1 1 d .
H1 H 0.7013 0.3684 0.7173 0.046 Uiso 1 1 calc R
C2 C 0.6293(6) 0.2371(5) 0.8009(4) 0.0466(13) Uani 1 1 d .
H2 H 0.7361 0.2499 0.8376 0.056 Uiso 1 1 calc R
C3 C 0.4926(6) 0.1494(5) 0.8190(4) 0.0396(11) Uani 1 1 d .
H3 H 0.5051 0.1026 0.8683 0.048 Uiso 1 1 calc R
C4 C 0.3340(6) 0.1316(4) 0.7619(3) 0.0348(11) Uani 1 1 d .
C5 C 0.1783(6) 0.0474(4) 0.7747(3) 0.0332(10) Uani 1 1 d .
C6 C 0.0283(6) 0.0407(4) 0.7177(3) 0.0313(10) Uani 1 1 d .
C7 C 0.0111(5) 0.1137(4) 0.6424(3) 0.0292(10) Uani 1 1 d .
C8 C -0.1398(5) 0.1108(4) 0.5820(3) 0.0346(11) Uani 1 1 d .
H8 H -0.2423 0.0573 0.5887 0.042 Uiso 1 1 calc R
C9 C -0.1338(6) 0.1869(5) 0.5140(4) 0.0375(11) Uani 1 1 d .
H9 H -0.2326 0.1877 0.4749 0.045 Uiso 1 1 calc R
C10 C 0.0212(6) 0.2638(5) 0.5031(4) 0.0362(11) Uani 1 1 d .
H10 H 0.0237 0.3134 0.4545 0.043 Uiso 1 1 calc R
C11 C 0.1634(5) 0.1945(4) 0.6281(3) 0.0286(10) Uani 1 1 d .
C12 C 0.3239(5) 0.2053(4) 0.6888(3) 0.0307(10) Uani 1 1 d .
C13 C -0.0092(6) -0.0898(5) 0.8216(4) 0.0385(11) Uani 1 1 d .
C14 C -0.1016(6) -0.1830(5) 0.8744(4) 0.0410(12) Uani 1 1 d .
C15 C -0.2682(7) -0.2357(6) 0.8641(4) 0.0622(16) Uani 1 1 d .
H15 H -0.3468 -0.2162 0.8199 0.075 Uiso 1 1 calc R
C16 C -0.3129(8) -0.3238(6) 0.9267(4) 0.0644(17) Uani 1 1 d .
H16 H -0.4231 -0.3691 0.9282 0.077 Uiso 1 1 calc R
C17 C -0.1769(7) -0.3335(5) 0.9834(4) 0.0486(13) Uani 1 1 d .
C18 C 0.2177(7) 0.5999(6) 0.7051(5) 0.0648(17) Uani 1 1 d .
H18A H 0.1648 0.6061 0.6388 0.097 Uiso 1 1 calc R
H18B H 0.2370 0.6896 0.7647 0.097 Uiso 1 1 calc R
H18C H 0.1455 0.5285 0.7250 0.097 Uiso 1 1 calc R
Cl1 Cl 0.45399(14) 0.18465(11) 0.39858(9) 0.0385(3) Uani 1 1 d .
Cl2 Cl 0.31244(14) 0.48456(11) 0.42722(9) 0.0375(3) Uani 1 1 d .
N1 N 0.4605(4) 0.2910(3) 0.6711(3) 0.0311(8) Uani 1 1 d .
N2 N 0.1661(4) 0.2694(4) 0.5591(3) 0.0321(8) Uani 1 1 d .
N3 N 0.1553(5) -0.0336(4) 0.8407(3) 0.0369(9) Uani 1 1 d .
N4 N -0.0929(5) -0.0483(4) 0.7487(3) 0.0353(9) Uani 1 1 d .
H4 H -0.1996 -0.0726 0.7264 0.042 Uiso 1 1 calc R
O1 O 0.3758(4) 0.5634(3) 0.6851(2) 0.0449(8) Uani 1 1 d .
H1A H 0.4389 0.6337 0.6752 0.054 Uiso 1 1 d R
S1 S 0.00864(17) -0.23597(14) 0.96458(11) 0.0504(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'
S S 0.1246 0.1234 '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'
Ni Ni 0.3393 1.1124 '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'
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
N2 Ni1 N1 80.32(13) . .
N2 Ni1 O1 91.01(13) . .
N1 Ni1 O1 90.15(12) . .
N2 Ni1 Cl2 173.11(10) . 2_666
N1 Ni1 Cl2 94.76(10) . 2_666
O1 Ni1 Cl2 84.14(9) . 2_666
N2 Ni1 Cl2 94.86(10) . .
N1 Ni1 Cl2 173.83(10) . .
O1 Ni1 Cl2 86.07(9) . .
Cl2 Ni1 Cl2 89.71(4) 2_666 .
N2 Ni1 Cl1 93.69(10) . .
N1 Ni1 Cl1 93.68(10) . .
O1 Ni1 Cl1 174.38(9) . .
Cl2 Ni1 Cl1 91.44(4) 2_666 .
Cl2 Ni1 Cl1 90.45(4) . .
N1 C1 C2 122.8(4) . .
N1 C1 H1 118.6 . .
C2 C1 H1 118.6 . .
C3 C2 C1 119.7(4) . .
C3 C2 H2 120.1 . .
C1 C2 H2 120.1 . .
C2 C3 C4 118.8(4) . .
C2 C3 H3 120.6 . .
C4 C3 H3 120.6 . .
C3 C4 C12 117.8(4) . .
C3 C4 C5 125.3(4) . .
C12 C4 C5 116.9(4) . .
C6 C5 N3 111.2(4) . .
C6 C5 C4 120.9(4) . .
N3 C5 C4 127.9(4) . .
C5 C6 N4 105.7(4) . .
C5 C6 C7 124.5(4) . .
N4 C6 C7 129.8(4) . .
C11 C7 C8 118.3(4) . .
C11 C7 C6 114.9(4) . .
C8 C7 C6 126.8(4) . .
C9 C8 C7 119.2(4) . .
C9 C8 H8 120.4 . .
C7 C8 H8 120.4 . .
C8 C9 C10 119.6(4) . .
C8 C9 H9 120.2 . .
C10 C9 H9 120.2 . .
N2 C10 C9 122.9(4) . .
N2 C10 H10 118.6 . .
C9 C10 H10 118.6 . .
N2 C11 C7 121.3(4) . .
N2 C11 C12 116.8(3) . .
C7 C11 C12 121.8(4) . .
N1 C12 C4 122.8(4) . .
N1 C12 C11 116.1(3) . .
C4 C12 C11 121.0(4) . .
N3 C13 N4 113.2(4) . .
N3 C13 C14 126.1(4) . .
N4 C13 C14 120.6(4) . .
C15 C14 C13 128.9(5) . .
C15 C14 S1 111.7(4) . .
C13 C14 S1 119.3(4) . .
C14 C15 C16 113.6(5) . .
C14 C15 H15 123.2 . .
C16 C15 H15 123.2 . .
C17 C16 C15 111.3(5) . .
C17 C16 H16 124.3 . .
C15 C16 H16 124.3 . .
C16 C17 S1 113.3(4) . .
C16 C17 Br1 126.4(4) . .
S1 C17 Br1 120.2(3) . .
O1 C18 H18A 109.5 . .
O1 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
O1 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
Ni1 Cl2 Ni1 90.29(4) 2_666 .
C1 N1 C12 118.1(4) . .
C1 N1 Ni1 128.6(3) . .
C12 N1 Ni1 113.3(3) . .
C10 N2 C11 118.7(4) . .
C10 N2 Ni1 128.0(3) . .
C11 N2 Ni1 113.3(3) . .
C13 N3 C5 103.9(4) . .
C13 N4 C6 105.9(4) . .
C13 N4 H4 127.0 . .
C6 N4 H4 127.0 . .
C18 O1 Ni1 124.5(3) . .
C18 O1 H1A 105.9 . .
Ni1 O1 H1A 105.9 . .
C17 S1 C14 90.1(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N2 2.056(3) .
Ni1 N1 2.069(3) .
Ni1 O1 2.150(3) .
Ni1 Cl2 2.4013(12) 2_666
Ni1 Cl2 2.4150(12) .
Ni1 Cl1 2.4375(13) .
Br1 C17 1.870(5) .
C1 N1 1.315(5) .
C1 C2 1.397(6) .
C1 H1 0.9300 .
C2 C3 1.370(6) .
C2 H2 0.9300 .
C3 C4 1.398(6) .
C3 H3 0.9300 .
C4 C12 1.402(5) .
C4 C5 1.437(6) .
C5 C6 1.368(6) .
C5 N3 1.373(5) .
C6 N4 1.378(5) .
C6 C7 1.430(6) .
C7 C11 1.407(5) .
C7 C8 1.409(6) .
C8 C9 1.353(6) .
C8 H8 0.9300 .
C9 C10 1.392(6) .
C9 H9 0.9300 .
C10 N2 1.330(5) .
C10 H10 0.9300 .
C11 N2 1.357(5) .
C11 C12 1.451(6) .
C12 N1 1.355(5) .
C13 N3 1.322(6) .
C13 N4 1.359(6) .
C13 C14 1.468(6) .
C14 C15 1.339(7) .
C14 S1 1.721(5) .
C15 C16 1.413(7) .
C15 H15 0.9300 .
C16 C17 1.334(7) .
C16 H16 0.9300 .
C17 S1 1.717(5) .
C18 O1 1.436(6) .
C18 H18A 0.9600 .
C18 H18B 0.9600 .
C18 H18C 0.9600 .
Cl2 Ni1 2.4013(12) 2_666
N4 H4 0.8600 .
O1 H1A 0.8500 .
