Structural Characterization of Thermochromic and Spin Equilibria in Solid-State Ni(detu)4Cl2 (detu = N,N'-Diethylthiourea).
Alfurayj, Ibrahim A.; Young, Jr, Victor G; Jensen, Michael P.; Inorganic chemistry 55 (2016) 1469–1479; doi:10.1021/acs.inorgchem.5b02203

data_4346833
_publ_section_title
;
 Structural Characterization of Thermochromic and Spin Equilibria in
 Solid-State Ni(detu)4Cl2 (detu = N,N'-Diethylthiourea).
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1469
_journal_page_last               1479
_journal_paper_doi               10.1021/acs.inorgchem.5b02203
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C20 H48 N8 Ni S4, 2(Cl)'
_chemical_formula_sum            'C20 H48 Cl2 N8 Ni S4'
_chemical_formula_weight         658.51
_chemical_name_systematic        Nidetu4Cl2_223K
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90.308(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4078(4)
_cell_length_b                   29.7627(14)
_cell_length_c                   10.5579(4)
_cell_measurement_reflns_used    2983
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      74.57
_cell_measurement_theta_min      2.97
_cell_volume                     3270.4(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker VENTURE PHOTON-100'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0795
_diffrn_reflns_av_unetI/netI     0.0630
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            28868
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.478
_diffrn_reflns_theta_min         2.969
_diffrn_source                   'ImuS microfocus'
_exptl_absorpt_coefficient_mu    4.933
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.4815
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/3 (Sheldrick, 2014)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.040
_exptl_transmission_factor_max   0.7538
_exptl_transmission_factor_min   0.4815
_refine_diff_density_max         0.704
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         6515
_refine_ls_number_restraints     238
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1057
_refine_ls_R_factor_gt           0.0768
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+18.0742P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1473
_refine_ls_wR_factor_ref         0.1614
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4658
_reflns_number_total             6515
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02203_si_001.cif
_cod_data_source_block           223K_Nidetu4Cl2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4346833
_shelx_estimated_absorpt_t_min   0.470
_shelx_estimated_absorpt_t_max   0.827
_shelxl_version_number           2014/6
_shelx_res_checksum              92264
_shelx_hkl_checksum              85930