Second-sphere hydrogen-bonding in heteroditopic mercaptopyridinium copper(I) frameworks
Bianketti, Sławomir; Blake, Alexander J.; Wilson, Claire; Hubberstey, Peter; Champness, Neil R.; Schröder, Martin; CrystEngComm 11 (2009) 763–; doi:10.1039/b813672f

data_7200369
_publ_section_title
;
 Second-sphere hydrogen-bonding in heteroditopic mercaptopyridinium
 copper(I) frameworks
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              763
_journal_paper_doi               10.1039/b813672f
_journal_volume                  11
_journal_year                    2009
_chemical_formula_moiety
'C65 H65 Cu6 N13 S13 6+, 2(Si F6 2-), 2(B F4 -), 7.5(C H4 O)'
_chemical_formula_sum            'C72.5 H95 B2 Cu6 F20 N13 O7.5 S13 Si2'
_chemical_formula_weight         2524.45
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'enCIFer editing of SHELXL97 CIF output'
_cell_angle_alpha                90.00
_cell_angle_beta                 97.551(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.242(5)
_cell_length_b                   15.310(3)
_cell_length_c                   28.120(6)
_cell_measurement_reflns_used    4298
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.0
_cell_measurement_theta_min      2.2
_cell_volume                     9919(4)
_computing_cell_refinement       'Bruker SAINT version 6.36A (Bruker, 2002)'
_computing_data_collection       'Bruker SMART version 5.624 (Bruker, 2001)'
_computing_data_reduction        'Bruker SAINT; SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics    ' ?'
_computing_publication_material
'enCIFer (Allen et al., 2004); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker SMART1000 CCD area detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.128
_diffrn_reflns_av_sigmaI/netI    0.244
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            53554
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         1.60
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.655
_exptl_absorpt_correction_T_max  0.624
_exptl_absorpt_correction_T_min  0.527
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Bruker SHELXTL; Bruker, 2001)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             5140
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.10
_refine_diff_density_min         -0.59
_refine_diff_density_rms         0.14
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.78
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1155
_refine_ls_number_reflns         22467
_refine_ls_number_restraints     425
_refine_ls_restrained_S_all      0.78
_refine_ls_R_factor_all          0.174
_refine_ls_R_factor_gt           0.0677
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.076P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.151
_refine_ls_wR_factor_ref         0.173
_reflns_number_gt                8414
_reflns_number_total             22467
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b813672f.txt
_cod_data_source_block           CUSPBF
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C72.50 H95 B2 Cu6 F20 N13 O7.50 S13 Si2'
_cod_database_code               7200369