Thermodynamics of the Cu(II) μ-Thiolate and Cu(I) Disulfide Equilibrium: A Combined Experimental and Theoretical Study.
Ording-Wenker, Erica C M; van der Plas, Martijn; Siegler, Maxime A.; Bonnet, Sylvestre; Bickelhaupt, F. Matthias; Fonseca Guerra, Célia; Bouwman, Elisabeth; Inorganic chemistry 53 (2014) 8494–8504; doi:10.1021/ic501060w

data_4340656
_publ_section_title
;
 Thermodynamics of the Cu(II) \m-Thiolate and Cu(I) Disulfide Equilibrium:
 A Combined Experimental and Theoretical Study.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8494
_journal_page_last               8504
_journal_paper_doi               10.1021/ic501060w
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C30 H36 Cu2 N6 S2, 2(B F4), C3 H6 O'
_chemical_formula_sum            'C33 H42 B2 Cu2 F8 N6 O S2'
_chemical_formula_weight         903.54
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
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_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.1268(2)
_cell_length_b                   10.28491(11)
_cell_length_c                   35.4103(4)
_cell_measurement_reflns_used    17365
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      71.87
_cell_measurement_theta_min      4.16
_cell_volume                     7694.21(14)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics    'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            27801
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.877
_diffrn_reflns_theta_min         4.185
_exptl_absorpt_coefficient_mu    3.045
_exptl_absorpt_correction_T_max  0.575
_exptl_absorpt_correction_T_min  0.392
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_description       block
_exptl_crystal_F_000             3696
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.355
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.13(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1111
_refine_ls_number_reflns         13538
_refine_ls_number_restraints     325
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0614P)^2^+12.2926P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1281
_refine_ls_wR_factor_ref         0.1291
_reflns_Friedel_coverage         0.966
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                13151
_reflns_number_total             13538
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic501060w_si_004.cif
_cod_data_source_block           '[CuII2(L2S)2](BF4)2_C3H6O'
_cod_depositor_comments
'Adding full bibliography for 4340656--4340658.cif.'
_cod_database_code               4340656
_shelxl_version_number           2013-2
_shelx_res_checksum              54929
_shelx_hkl_checksum              42587