Metal to Ligand Interactions and Hydrogen Bonding in the Design of Metallosupramolecular Compounds: Effect of pH and Aprotic Solvents on the Nature of Materials Based on Bis(4-pyridylthio)methane and Copper(II) Chloride
Lago, Ana Belén; Carballo, Rosa; García-Martínez, Emilia; Vázquez-López, Ezequiel M.; Crystal Growth & Design 11 (2011) 59–; doi:10.1021/cg1004566

data_4500091
_publ_section_title
;
 Metal to Ligand Interactions and Hydrogen Bonding in the Design of
 Metallosupramolecular Compounds: Effect of pH and Aprotic Solvents on the
 Nature of Materials Based on Bis(4-pyridylthio)methane and Copper(II)
 Chloride
;
_journal_issue                   1
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              59
_journal_paper_doi               10.1021/cg1004566
_journal_volume                  11
_journal_year                    2011
_chemical_formula_sum            'C22 H22 Cl4 Cu N4 O0 S4'
_chemical_formula_weight         676.02
_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                 92.112(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4580(16)
_cell_length_b                   14.530(2)
_cell_length_c                   18.410(3)
_cell_measurement_reflns_used    946
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      38.714
_cell_measurement_theta_min      4.801
_cell_volume                     2795.6(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker ORTEPIII and PLATON'
_computing_publication_material  'Bruker SHELX97'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0869
_diffrn_reflns_av_sigmaI/netI    0.1435
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            8921
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.01
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    1.483
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8571
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1372
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       0.0017(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         3321
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.1748
_refine_ls_R_factor_gt           0.0540
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0685P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1187
_refine_ls_wR_factor_ref         0.1723
_reflns_number_gt                1434
_reflns_number_total             3321
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg1004566_si_002.cif
_cod_data_source_block           3
_cod_original_cell_volume        2795.4(7)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4500091