Polymorph transformation in a mixed-stacking nickel-dithiolene complex with the derivative of 4,4'-bipyridinium.
Gao, Yan; Xu, Lei; Feng, Zi-Heng; Qian, Yin; Tian, Zheng-Fang; Ren, Xiao-Ming; Dalton transactions (Cambridge, England : 2003) 53 (2024) 8202–8213; doi:10.1039/d4dt00324a

data_7715756
_publ_section_title
;
 Polymorph transformation in a mixed-stacking nickel-dithiolene complex
 with the derivative of 4,4'-bipyridinium.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8202
_journal_page_last               8213
_journal_paper_doi               10.1039/d4dt00324a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         '2(C4 N2 Ni0.5 S2), 2(C9 H13 N)'
_chemical_formula_sum            'C26 H26 N6 Ni S4'
_chemical_formula_weight         609.48
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-04-14
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-04-15 deposited with the CCDC.	2024-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                94.597(3)
_cell_angle_beta                 94.082(3)
_cell_angle_gamma                93.219(3)
_cell_formula_units_Z            2
_cell_length_a                   7.1650(7)
_cell_length_b                   9.2160(8)
_cell_length_c                   21.1039(18)
_cell_measurement_reflns_used    6105
_cell_measurement_temperature    105(2)
_cell_measurement_theta_max      26.359
_cell_measurement_theta_min      2.348
_cell_volume                     1382.9(2)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      105.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_av_unetI/netI     0.0732
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            15728
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.405
_diffrn_reflns_theta_min         2.221
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.031
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5700
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1206 before and 0.0652 after correction.
The Ratio of minimum to maximum transmission is 0.7647.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_description       needle
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.663
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         5634
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+0.4941P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1116
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4277
_reflns_number_total             5634
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00324a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7715756--7715757.cif.'
_cod_database_code               7715756
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.904
_shelx_estimated_absorpt_t_min   0.683
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C23(H23A,H23B), C24(H24A,
 H24B), C25(H25A,H25B)
2.b Me refined with riding coordinates:
 C17(H17A,H17B,H17C), C26(H26A,H26B,H26C)
2.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C12(H12), C13(H13), C18(H18), C19(H19), C21(H21), C22(H22)
;
_shelx_res_checksum              28135
_olex2_submission_special_instructions 'No special instructions were received'