Ionic Crystals of {[Ni(phen)3]2Ge4S10}.xSol, Showing Solid-State Solvatochromism and Rapid Solvent-Induced Recrystallization
Wen-Qin Mu; Qin-Yu Zhu; Li-Sheng You; Xu Zhang; Wen Luo; Guo-Qing Bian; Jie Dai; Inorganic Chemistry 51 (2012) 1330–1335; doi:10.1021/ic2014682

data_4328118
_publ_section_title
;
 Ionic Crystals of {[Ni(phen)3]2Ge4S10}.xSol, Showing Solid-State
 Solvatochromism and Rapid Solvent-Induced Recrystallization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1330
_journal_page_last               1335
_journal_paper_doi               10.1021/ic2014682
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C75.5 H87.75 Ge4 N12 Ni2 O16.5 S10'
_chemical_formula_weight         2155.70
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 121.731(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   45.425(4)
_cell_length_b                   18.7598(13)
_cell_length_c                   24.955(2)
_cell_measurement_reflns_used    37060
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     18087(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0665
_diffrn_reflns_av_sigmaI/netI    0.0815
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            44101
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    2.020
_exptl_absorpt_correction_T_max  0.817
_exptl_absorpt_correction_T_min  0.498
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication '
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_description       Prism
_exptl_crystal_F_000             8806
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.927
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1068
_refine_ls_number_reflns         15851
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.1293
_refine_ls_R_factor_gt           0.1045
_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/[\s^2^(Fo^2^)+(0.0007P)^2^+372.8227P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1845
_refine_ls_wR_factor_ref         0.1956
_reflns_number_gt                12587
_reflns_number_total             15851
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2014682_si_002_1.cif
_cod_data_source_block           l
_cod_depositor_comments
;

2021-04-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         4311.41
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_Hall     '-C 2yc   '
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_original_formula_sum        'C151 H175.50 Ge8 N24 Ni4 O33 S20'
_cod_database_code               4328118