Kinetics Aspects of the Reversible Assembly of Copper in Heterometallic Mo<sub>3</sub>CuS<sub>4</sub> Clusters with 4,4'-Di-tert-butyl-2,2'-bipyridine.
Pino-Chamorro, Jose Ángel; Laricheva, Yuliya A.; Guillamón, Eva; Fernández-Trujillo, M Jesús; Algarra, Andrés G; Gushchin, Artem L.; Abramov, Pavel A.; Bustelo, Emilio; Llusar, Rosa; Sokolov, Maxim N.; Basallote, Manuel G.; Inorganic chemistry 55 (2016) 9912–9922; doi:10.1021/acs.inorgchem.6b01878

data_4349060
_publ_section_title
;
 Kinetics Aspects of the Reversible Assembly of Copper in Heterometallic
 Mo<sub>3</sub>CuS<sub>4</sub> Clusters with
 4,4'-Di-tert-butyl-2,2'-bipyridine.
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9912
_journal_page_last               9922
_journal_paper_doi               10.1021/acs.inorgchem.6b01878
_journal_volume                  55
_journal_year                    2016
_chemical_formula_structural     '[Mo3S4{CuCl}(N2C8(C4H9)2)3Cl3][CuCl2]*2CH2Cl2'
_chemical_formula_sum            'C54 H72 Cl6 Cu2 Mo3 N6 S4'
_chemical_formula_weight         1561.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 104.825(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.1480(16)
_cell_length_b                   19.0085(18)
_cell_length_c                   24.8846(19)
_cell_measurement_reflns_used    8430
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.54
_cell_measurement_theta_min      2.46
_cell_volume                     7841.3(12)
_computing_cell_refinement       'SAINT (Bruker-AXS, 2004)'
_computing_data_collection       'APEX2 (Bruker-AXS, 2004)'
_computing_data_reduction        'SAINT (Bruker-AXS, 2004)'
_computing_molecular_graphics    'SHELXLE (Sheldrick, 2011)'
_computing_publication_material  'CIFTAB-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker Nonius X8Apex CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0636
_diffrn_reflns_av_unetI/netI     0.0748
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            48644
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.741
_diffrn_reflns_theta_min         1.630
_exptl_absorpt_coefficient_mu    1.344
_exptl_absorpt_correction_T_max  0.900
_exptl_absorpt_correction_T_min  0.730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS, 2004)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_description       needle
_exptl_crystal_F_000             3152
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.376
_refine_diff_density_min         -0.939
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     670
_refine_ls_number_reflns         14768
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_gt           0.0597
_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^)+(0.1090P)^2^+3.9327P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1778
_refine_ls_wR_factor_ref         0.2018
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9283
_reflns_number_total             14768
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic6b01878_si_002.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4349060
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.730
_shelx_estimated_absorpt_t_max   0.900
_shelx_res_checksum              44066
_shelx_hkl_checksum              4889
_shelx_fab_checksum              7179