Ligand-forced dimerization of copper(I)‒olefin complexes bearing a 1,3,4-thiadiazole core
Ardan, Bohdan; Kinzhybalo, Vasyl; Slyvka, Yurii; Shyyka, Olga; Luk`yanov, Mykhaylo; Lis, Tadeusz; Mys`kiv, Marian; Acta Crystallographica Section C 73 (2017) 36–46; doi:10.1107/S2053229616018751

data_2020693
_publ_section_title
;
 Ligand-forced dimerization of copper(I)--olefin complexes bearing a
 1,3,4-thiadiazole core
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              36
_journal_page_last               46
_journal_paper_doi               10.1107/S2053229616018751
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac
'[Cu2 (Si F6) (C5 H7 N3 S2)2 (H2 O)], 0.5C2 H3 N, 2H2 O'
_chemical_formula_moiety
'C10 H140 Cu2 F6 N6 O1 S4 Si, 0.5(C2 H3 N), 2(H2 O)'
_chemical_formula_sum            'C11 H19.5 Cu2 F6 N6.5 O3 S4 Si'
_chemical_formula_weight         688.24
_chemical_name_systematic
;\m-Aqua-(hexafluorosilicato)bis{\m-5-[(prop-2-en-1-yl)sulfanyl]-1,3,4-thiadiazol-2-amine}dicopper(I) acetonitrile hemisolvate
dihydrate
;
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.04(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.899(4)
_cell_length_b                   11.442(4)
_cell_length_c                   17.678(5)
_cell_measurement_reflns_used    9071
_cell_measurement_temperature    260(2)
_cell_measurement_theta_max      36.7964
_cell_measurement_theta_min      2.9064
_cell_volume                     2353.9(13)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2010)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2010)
;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction, 2010)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      260.15
_diffrn_detector_area_resol_mean 8.3359
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Xcalibur Sapphire2 (large Be window)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24572
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.998
_diffrn_reflns_theta_min         2.912
_exptl_absorpt_coefficient_mu    2.289
_exptl_absorpt_correction_T_max  0.825
_exptl_absorpt_correction_T_min  0.452
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[CrysAlis PRO (Rigaku OD, 2015), based on expressions
derived by Clark & Reid (1995)]
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_description       prism
_exptl_crystal_F_000             1380
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.379
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         5649
_refine_ls_number_restraints     245
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0369
_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^)+(0.0420P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0869
_reflns_number_gt                3717
_reflns_number_total             5649
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fn3225sup1.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 2020689--2020694.cif.'
_cod_original_formula_sum        'C11 H19.50 Cu2 F6 N6.50 O3 S4 Si'
_cod_database_code               2020693
_cod_database_fobs_code          2020693
_shelx_estimated_absorpt_t_min   0.382
_shelx_estimated_absorpt_t_max   0.820
_shelx_hkl_checksum              30398
_shelx_res_checksum              89072