#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:41:30 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179419 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/16/4331616.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_4331616
loop_
_publ_author_name
'Ramababu Bolligarla'
'Samala Nagaprasad Reddy'
'Gummadi Durgaprasad'
'Vudagandla Sreenivasulu'
'Samar K. Das'
_publ_contact_author_address
; 
School of Chemistry
University of Hyderabad
Hyderabad 500 046,
India
;
_publ_contact_author_email       skdsc@uohyd.ernet.in
_publ_contact_author_name
;
Dr. Samar K. Das
;
_publ_contact_author_phone       +91-40-23011007
_publ_section_title
;
 Influence of the Substituents on the Electronic and Electrochemical
 Properties of a New Square-Planar Nickel-Bis(quinoxaline-6,7-dithiolate)
 System: Synthesis, Spectroscopy, Electrochemistry, Crystallography, and
 Theoretical Investigation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              66
_journal_page_last               76
_journal_paper_doi               10.1021/ic301017g
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C16 H4 Cl4 N4 Ni S4, 2(C16 H36 N)'
_chemical_formula_sum            'C48 H76 Cl4 N6 Ni S4'
_chemical_formula_weight         1065.94
_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                 101.239(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.8484(15)
_cell_length_b                   8.5484(9)
_cell_length_c                   22.521(3)
_cell_measurement_reflns_used    3342
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.42
_cell_measurement_theta_min      2.55
_cell_volume                     2614.9(5)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0771
_diffrn_reflns_av_sigmaI/netI    0.0584
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            23914
_diffrn_reflns_theta_full        24.94
_diffrn_reflns_theta_max         24.94
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    0.771
_exptl_absorpt_correction_T_max  0.9552
_exptl_absorpt_correction_T_min  0.8366
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_description       block
_exptl_crystal_F_000             988
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.377
_refine_diff_density_min         -0.791
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.249
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         4580
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.249
_refine_ls_R_factor_all          0.1830
_refine_ls_R_factor_gt           0.1690
_refine_ls_shift/su_max          0.058
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1201P)²+34.3639P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3640
_refine_ls_wR_factor_ref         0.3733
_reflns_number_gt                4019
_reflns_number_total             4580
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301017g_si_002_4.cif
_cod_data_source_block           compound3
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               4331616
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
C13 C 0.671(3) 0.619(6) 0.8939(12) 0.21(2) Uani 1 1 d .
Ni1 Ni 1.0000 1.0000 0.0000 0.0298(5) Uani 1 2 d S
S1 S 0.8427(2) 1.0378(3) -0.02368(12) 0.0353(7) Uani 1 1 d .
Cl2 Cl 0.5514(3) 0.6721(7) 0.23356(17) 0.0936(17) Uani 1 1 d .
N1 N 0.5623(7) 0.9057(14) 0.0841(5) 0.056(3) Uani 1 1 d .
C3 C 0.8245(9) 0.8099(17) 0.1284(5) 0.053(3) Uani 1 1 d .
H3 H 0.8672 0.7577 0.1590 0.064 Uiso 1 1 calc R
C1 C 0.7942(8) 0.9559(13) 0.0349(5) 0.038(3) Uani 1 1 d .
C2 C 0.8603(8) 0.8774(14) 0.0828(5) 0.041(3) Uani 1 1 d .
C4 C 0.7249(9) 0.8176(17) 0.1299(5) 0.051(3) Uani 1 1 d .
N2 N 0.6893(8) 0.7498(16) 0.1767(5) 0.064(3) Uani 1 1 d .
C5 C 0.6593(8) 0.8957(15) 0.0834(5) 0.045(3) Uani 1 1 d .
C6 C 0.6975(9) 0.9651(15) 0.0367(5) 0.046(3) Uani 1 1 d .
H6 H 0.6554 1.0187 0.0063 0.056 Uiso 1 1 calc R
C7 C 0.5957(10) 0.758(2) 0.1741(6) 0.064(4) Uani 1 1 d .
C8 C 0.5321(9) 0.8397(19) 0.1279(6) 0.059(4) Uani 1 1 d .
N3 N 0.7737(9) 0.5780(13) 0.8838(5) 0.067(4) Uani 1 1 d .
C18 C 0.815(2) 0.504(4) 0.9959(10) 0.170(15) Uani 1 1 d .
C19 C 0.8788(10) 0.4436(18) 1.0484(7) 0.063(4) Uani 1 1 d .
C12 C 0.9791(19) 0.923(4) 0.7762(12) 0.140(11) Uani 1 1 d .
C9 C 0.793(4) 0.731(3) 0.8501(18) 0.26(3) Uani 1 1 d .
C10 C 0.8832(12) 0.729(4) 0.8450(17) 0.182(19) Uani 1 1 d .
C11 C 0.900(4) 0.873(4) 0.8025(12) 0.22(2) Uani 1 1 d .
C17 C 0.8256(15) 0.538(5) 0.9439(12) 0.24(2) Uani 1 1 d .
Cl3 Cl 0.4050(3) 0.8538(5) 0.12648(19) 0.0783(13) Uani 1 1 d .
S2 S 0.9848(2) 0.8654(4) 0.07881(13) 0.0459(8) Uani 1 1 d .
C23 C 0.771(2) 0.269(3) 0.7595(13) 0.142(11) Uani 1 1 d .
C21 C 0.7691(19) 0.451(3) 0.8413(16) 0.176(16) Uani 1 1 d .
C20 C 0.839(2) 0.377(3) 1.0996(14) 0.148(11) Uani 1 1 d .
C15 C 0.528(2) 0.716(4) 0.9257(19) 0.192(17) Uani 1 1 d .
C16 C 0.449(2) 0.651(4) 0.9240(19) 0.183(16) Uani 1 1 d .
C14 C 0.6220(16) 0.664(6) 0.9156(14) 0.20(2) Uani 1 1 d .
C24 C 0.715(2) 0.225(6) 0.721(2) 0.28(3) Uani 1 1 d .
C22 C 0.766(3) 0.408(3) 0.7948(12) 0.21(2) 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'
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'
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
C14 C13 N3 156(5) . .
S2 Ni1 S2 179.998(1) . 3_775
S2 Ni1 S1 88.42(10) . 3_775
S2 Ni1 S1 91.58(10) 3_775 3_775
S2 Ni1 S1 91.58(10) . .
S2 Ni1 S1 88.42(10) 3_775 .
S1 Ni1 S1 180.0 3_775 .
C1 S1 Ni1 105.8(4) . .
C8 N1 C5 117.3(12) . .
C2 C3 C4 120.7(12) . .
C2 C3 H3 119.6 . .
C4 C3 H3 119.6 . .
C6 C1 C2 119.7(10) . .
C6 C1 S1 122.1(9) . .
C2 C1 S1 118.2(8) . .
C3 C2 C1 119.7(11) . .
C3 C2 S2 121.6(10) . .
C1 C2 S2 118.7(8) . .
N2 C4 C3 120.4(12) . .
N2 C4 C5 119.5(11) . .
C3 C4 C5 120.1(11) . .
C7 N2 C4 116.7(12) . .
N1 C5 C6 120.4(11) . .
N1 C5 C4 121.1(11) . .
C6 C5 C4 118.4(11) . .
C1 C6 C5 121.4(11) . .
C1 C6 H6 119.3 . .
C5 C6 H6 119.3 . .
N2 C7 C8 122.6(12) . .
N2 C7 Cl2 116.4(12) . .
C8 C7 Cl2 121.0(10) . .
N1 C8 C7 122.6(12) . .
N1 C8 Cl3 115.7(11) . .
C7 C8 Cl3 121.7(10) . .
C17 N3 C21 113(3) . .
C17 N3 C9 124(2) . .
C21 N3 C9 107(2) . .
C17 N3 C13 103.0(16) . .
C21 N3 C13 111(2) . .
C9 N3 C13 98(2) . .
C17 C18 C19 134(2) . .
C18 C19 C20 121(2) . .
C10 C9 N3 107(3) . .
C9 C10 C11 107(4) . .
C12 C11 C10 134(4) . .
C18 C17 N3 144(2) . .
C2 S2 Ni1 105.4(4) . .
C24 C23 C22 128(4) . .
C22 C21 N3 151(4) . .
C16 C15 C14 133(4) . .
C13 C14 C15 158(5) . .
C21 C22 C23 143(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C13 C14 0.98(4) .
C13 N3 1.53(4) .
Ni1 S2 2.160(3) .
Ni1 S2 2.160(3) 3_775
Ni1 S1 2.163(3) 3_775
Ni1 S1 2.163(3) .
S1 C1 1.741(11) .
Cl2 C7 1.740(13) .
N1 C8 1.274(17) .
N1 C5 1.350(15) .
C3 C2 1.353(16) .
C3 C4 1.389(17) .
C3 H3 0.9300 .
C1 C6 1.350(16) .
C1 C2 1.436(16) .
C2 S2 1.747(11) .
C4 N2 1.374(15) .
C4 C5 1.414(18) .
N2 C7 1.289(17) .
C5 C6 1.397(16) .
C6 H6 0.9300 .
C7 C8 1.41(2) .
C8 Cl3 1.758(13) .
N3 C17 1.44(2) .
N3 C21 1.44(2) .
N3 C9 1.56(5) .
C18 C17 1.24(3) .
C18 C19 1.43(2) .
C19 C20 1.48(2) .
C12 C11 1.41(4) .
C9 C10 1.28(6) .
C10 C11 1.60(5) .
C23 C24 1.11(4) .
C23 C22 1.44(3) .
C21 C22 1.10(3) .
C15 C16 1.21(4) .
C15 C14 1.44(4) .
