#------------------------------------------------------------------------------
#$Date: 2021-02-05 01:15:53 +0200 (Fri, 05 Feb 2021) $
#$Revision: 261679 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/60/7706007.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_7706007
loop_
_publ_author_name
'Bilyj, Jessica K.'
'Silajew, Nicole V.'
'Bernhardt, Paul V.'
_publ_section_title
;
 Nickel coordination chemistry of bis(dithiocarbazate) Schiff base
 ligands; metal and ligand centred redox reactions.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              612
_journal_page_last               623
_journal_paper_doi               10.1039/d0dt03204b
_journal_volume                  50
_journal_year                    2021
_chemical_formula_sum            'C9 H14 N4 Ni S4'
_chemical_formula_weight         365.19
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.5
_audit_creation_date             2020-09-14T12:29:04-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2020-10-24 deposited with the CCDC.	2020-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                104.320(8)
_cell_angle_beta                 104.614(8)
_cell_angle_gamma                96.573(8)
_cell_formula_units_Z            2
_cell_length_a                   7.6588(7)
_cell_length_b                   8.7590(10)
_cell_length_c                   11.3774(9)
_cell_measurement_reflns_used    2289
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      62.6
_cell_measurement_theta_min      5.3
_cell_measurement_wavelength     0.71073
_cell_volume                     702.75(13)
_computing_cell_refinement       'CrysalisPro (Agilent Technologies,     )'
_computing_data_collection       'CrysalisPro (Agilent Technologies,     )'
_computing_data_reduction        'CrysalisPro (Agilent Technologies,     )'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      190(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.02
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type
'Agilent Technologies Xcalibur, EosS2, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.078025
_diffrn_orient_matrix_UB_12      -0.179984
_diffrn_orient_matrix_UB_13      -0.030115
_diffrn_orient_matrix_UB_21      0.191823
_diffrn_orient_matrix_UB_22      -0.027438
_diffrn_orient_matrix_UB_23      0.063928
_diffrn_orient_matrix_UB_31      -0.043826
_diffrn_orient_matrix_UB_32      0.032025
_diffrn_orient_matrix_UB_33      0.12785
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4193
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_reduction_process
;
 Scaled and merged with Sortav
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        62.392
_diffrn_reflns_theta_max         62.392
_diffrn_reflns_theta_min         4.192
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.442
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
        Empirical absorption correction using spherical harmonics,
        implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.874
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     167
_refine_ls_number_reflns         2211
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0752P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.115
_refine_ls_wR_factor_ref         0.1196
_reflns_Friedel_coverage         0
_reflns_number_gt                2000
_reflns_number_total             2211
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt03204b2.cif
_cod_data_source_block           1817jb21
_cod_depositor_comments
'Adding full bibliography for 7706005--7706008.cif.'
_cod_original_cell_volume        702.75(12)
_cod_database_code               7706007
_shelx_shelxl_version_number     2018/1
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4085(4) 0.9026(4) 0.6689(3) 0.0306(7) Uani 1 1 d . . . . .
C2 C 0.3259(4) 1.2222(4) 0.5635(3) 0.0312(7) Uani 1 1 d . . . . .
C3 C 0.2232(5) 1.2741(4) 0.4552(3) 0.0336(7) Uani 1 1 d . . . . .
H3A H 0.147652 1.348169 0.489241 0.04 Uiso 1 1 calc R U . . .
H3B H 0.316153 1.339719 0.432176 0.04 Uiso 1 1 calc R U . . .
C4 C 0.1000(4) 1.1626(4) 0.3339(3) 0.0320(7) Uani 1 1 d . . . . .
C5 C -0.0814(4) 0.7724(4) 0.1748(3) 0.0291(7) Uani 1 1 d . . . . .
C6 C 0.6513(5) 1.0314(4) 0.9085(3) 0.0416(8) Uani 1 1 d . . . . .
H6A H 0.731429 1.0862 0.870739 0.062 Uiso 1 1 calc R U . . .
H6B H 0.725787 1.012998 0.985709 0.062 Uiso 1 1 calc R U . . .
H6C H 0.562991 1.098079 0.929843 0.062 Uiso 1 1 calc R U . . .
C7 C 0.4411(5) 1.3566(4) 0.6766(3) 0.0368(8) Uani 1 1 d . . . . .
H7A H 0.399329 1.352895 0.750618 0.055 Uiso 1 1 calc R U . . .
H7B H 0.428893 1.459615 0.659104 0.055 Uiso 1 1 calc R U . . .
H7C H 0.570108 1.345027 0.69369 0.055 Uiso 1 1 calc R U . . .
C8 C 0.0146(5) 1.2414(5) 0.2374(3) 0.0411(8) Uani 1 1 d . . . . .
H8A H 0.05137 1.202809 0.160442 0.062 Uiso 1 1 calc R U . . .
H8B H 0.055692 1.357914 0.271417 0.062 Uiso 1 1 calc R U . . .
H8C H -0.119508 1.215155 0.216981 0.062 Uiso 1 1 calc R U . . .
C9 C -0.2412(5) 0.4571(4) 0.0267(3) 0.0416(8) Uani 1 1 d . . . . .
H9A H -0.11581 0.43581 0.044187 0.062 Uiso 1 1 calc R U . . .
H9B H -0.315719 0.386613 -0.056447 0.062 Uiso 1 1 calc R U . . .
H9C H -0.294979 0.43673 0.092249 0.062 Uiso 1 1 calc R U . . .
N1 N 0.4235(4) 1.0504(3) 0.6734(2) 0.0317(6) Uani 1 1 d . . . . .
N2 N 0.3143(3) 1.0736(3) 0.5602(2) 0.0293(6) Uani 1 1 d . . . . .
N3 N 0.0688(3) 1.0091(3) 0.3144(2) 0.0285(6) Uani 1 1 d . . . . .
N4 N -0.0562(4) 0.9249(4) 0.1944(3) 0.0338(6) Uani 1 1 d . . . . .
S1 S 0.27577(11) 0.74310(10) 0.54079(7) 0.0328(3) Uani 1 1 d . . . . .
S2 S 0.02538(11) 0.67660(10) 0.28081(7) 0.0339(2) Uani 1 1 d . . . . .
S3 S 0.52939(11) 0.84192(10) 0.79716(7) 0.0353(3) Uani 1 1 d . . . . .
S4 S -0.23617(11) 0.66368(10) 0.02721(7) 0.0386(3) Uani 1 1 d . . . . .
Ni1 Ni 0.17329(6) 0.89252(6) 0.42515(4) 0.0271(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 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 '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
N1 C1 S1 125.6(3) . . ?
N1 C1 S3 121.0(2) . . ?
S1 C1 S3 113.4(2) . . ?
N2 C2 C3 122.1(3) . . ?
N2 C2 C7 123.0(3) . . ?
C3 C2 C7 114.8(3) . . ?
C4 C3 C2 124.3(3) . . ?
N3 C4 C3 122.3(3) . . ?
N3 C4 C8 122.7(3) . . ?
C3 C4 C8 115.1(3) . . ?
N4 C5 S2 124.6(2) . . ?
N4 C5 S4 114.1(2) . . ?
S2 C5 S4 121.3(2) . . ?
C1 N1 N2 112.1(3) . . ?
C2 N2 N1 113.0(3) . . ?
C2 N2 Ni1 127.5(2) . . ?
N1 N2 Ni1 119.5(2) . . ?
C4 N3 N4 113.4(3) . . ?
C4 N3 Ni1 127.3(2) . . ?
N4 N3 Ni1 119.3(2) . . ?
C5 N4 N3 112.7(3) . . ?
C1 S1 Ni1 94.68(12) . . ?
C5 S2 Ni1 95.34(11) . . ?
C1 S3 C6 101.69(17) . . ?
C5 S4 C9 103.86(17) . . ?
N3 Ni1 N2 96.42(12) . . ?
N3 Ni1 S2 88.07(8) . . ?
N2 Ni1 S2 175.46(9) . . ?
N3 Ni1 S1 175.32(9) . . ?
N2 Ni1 S1 88.14(9) . . ?
S2 Ni1 S1 87.38(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
C1 N1 1.273(4) . ?
C1 S1 1.741(3) . ?
C1 S3 1.756(3) . ?
C2 N2 1.285(4) . ?
C2 C3 1.488(5) . ?
C2 C7 1.504(5) . ?
C3 C4 1.488(5) . ?
C4 N3 1.290(4) . ?
C4 C8 1.492(5) . ?
C5 N4 1.281(5) . ?
C5 S2 1.729(3) . ?
C5 S4 1.755(3) . ?
C6 S3 1.800(4) . ?
C9 S4 1.804(4) . ?
N1 N2 1.422(4) . ?
N2 Ni1 1.899(3) . ?
N3 N4 1.416(4) . ?
N3 Ni1 1.894(3) . ?
S1 Ni1 2.1508(9) . ?
S2 Ni1 2.1427(9) . ?
