#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:21:06 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180334 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/03/7200366.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7200366
loop_
_publ_author_name
'Bianketti, Sławomir'
'Blake, Alexander J.'
'Wilson, Claire'
'Hubberstey, Peter'
'Champness, Neil R.'
'Schröder, Martin'
_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         'C30 H30 Cu2 N6 S6, 2(Cl)'
_chemical_formula_sum            'C30 H30 Cl2 Cu2 N6 S6'
_chemical_formula_weight         865.02
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 100.205(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.4535(15)
_cell_length_b                   7.3436(8)
_cell_length_c                   17.428(2)
_cell_measurement_reflns_used    2597
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.45
_cell_measurement_theta_min      2.85
_cell_volume                     1820.6(3)
_computing_cell_refinement       'Bruker SAINT version 6.36a (Bruker, 2002)'
_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)'
_computing_molecular_graphics    ' ?'
_computing_publication_material
'enCIFer(Allen et al.,2004);PLATON (Spek,2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'WinGX - Version 1.70.01; SIR-92'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.047
_diffrn_reflns_av_sigmaI/netI    0.0521
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9586
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.69
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.691
_exptl_absorpt_correction_T_max  0.919
_exptl_absorpt_correction_T_min  0.799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SHELXTL; Bruker, 2001)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.42
_refine_diff_density_min         -0.29
_refine_diff_density_rms         0.07
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.912
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3205
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.912
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0288
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0224P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0536
_refine_ls_wR_factor_ref         0.0578
_reflns_number_gt                2261
_reflns_number_total             3205
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b813672f.txt
_cod_data_source_block           compound_1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7200366
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu Cu 0.00859(2) 0.00312(5) 0.596296(19) 0.02619(11) Uani 1 1 d . . .
S34 S 0.14540(5) -0.06948(11) 0.67994(4) 0.0299(2) Uani 1 1 d . . .
S24 S 0.03667(5) 0.22444(10) 0.49910(4) 0.02518(18) Uani 1 1 d . . .
S14 S -0.10733(5) 0.06673(11) 0.66666(4) 0.02875(19) Uani 1 1 d . . .
C23 C 0.2115(2) 0.2573(4) 0.45897(16) 0.0291(7) Uani 1 1 d . . .
H23 H 0.1825 0.2351 0.4065 0.035 Uiso 1 1 calc R . .
C14 C -0.09875(17) 0.2831(4) 0.70317(15) 0.0226(7) Uani 1 1 d . . .
C13 C -0.04312(19) 0.4193(4) 0.67786(16) 0.0276(7) Uani 1 1 d . . .
H13 H -0.0094 0.3931 0.6371 0.033 Uiso 1 1 calc R . .
C32 C 0.2836(2) -0.2318(4) 0.51183(17) 0.0316(8) Uani 1 1 d . . .
H32 H 0.2710 -0.2497 0.4570 0.038 Uiso 1 1 calc R . .
C24 C 0.15558(19) 0.2662(4) 0.51740(16) 0.0248(7) Uani 1 1 d . . .
N11 N -0.08486(16) 0.6284(3) 0.76736(14) 0.0332(6) Uani 1 1 d . . .
H11 H -0.0792 0.7375 0.7886 0.040 Uiso 1 1 calc R . .
C22 C 0.3060(2) 0.2799(4) 0.47648(18) 0.0347(8) Uani 1 1 d . . .
H22 H 0.3426 0.2729 0.4364 0.042 Uiso 1 1 calc R . .
C33 C 0.21380(19) -0.1729(4) 0.54862(16) 0.0283(7) Uani 1 1 d . . .
H33 H 0.1530 -0.1508 0.5191 0.034 Uiso 1 1 calc R . .
C34 C 0.23014(19) -0.1439(4) 0.63006(16) 0.0254(7) Uani 1 1 d . . .
C26 C 0.2977(2) 0.3304(4) 0.60739(17) 0.0346(8) Uani 1 1 d . . .
H26 H 0.3287 0.3574 0.6589 0.042 Uiso 1 1 calc R . .
N21 N 0.34796(16) 0.3123(3) 0.55043(15) 0.0356(7) Uani 1 1 d . . .
H21 H 0.4096 0.3217 0.5615 0.043 Uiso 1 1 calc R . .
C15 C -0.14977(19) 0.3360(4) 0.76143(16) 0.0306(7) Uani 1 1 d . . .
H15 H -0.1907 0.2509 0.7793 0.037 Uiso 1 1 calc R . .
C25 C 0.2032(2) 0.3109(4) 0.59269(16) 0.0298(7) Uani 1 1 d . . .
H25 H 0.1685 0.3275 0.6336 0.036 Uiso 1 1 calc R . .
C16 C -0.1415(2) 0.5055(5) 0.79229(17) 0.0345(8) Uani 1 1 d . . .
H16 H -0.1761 0.5377 0.8318 0.041 Uiso 1 1 calc R . .
C12 C -0.0364(2) 0.5872(4) 0.71028(17) 0.0316(7) Uani 1 1 d . . .
H12 H 0.0025 0.6766 0.6927 0.038 Uiso 1 1 calc R . .
C36 C 0.3899(2) -0.2400(4) 0.62981(19) 0.0391(8) Uani 1 1 d . . .
H36 H 0.4515 -0.2642 0.6574 0.047 Uiso 1 1 calc R . .
N31 N 0.37011(17) -0.2650(3) 0.55186(15) 0.0355(7) Uani 1 1 d . . .
H31 H 0.4144 -0.3035 0.5271 0.043 Uiso 1 1 calc R . .
C35 C 0.3229(2) -0.1807(4) 0.66889(18) 0.0360(8) Uani 1 1 d . . .
H35 H 0.3384 -0.1634 0.7237 0.043 Uiso 1 1 calc R . .
Cl Cl 0.55777(5) 0.41742(11) 0.59957(4) 0.03034(19) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S14 Cu S34 109.61(3) . . ?
S14 Cu S24 112.49(3) . 3_556 ?
S34 Cu S24 112.39(3) . 3_556 ?
S14 Cu S24 117.65(3) . . ?
S34 Cu S24 111.41(3) . . ?
S24 Cu S24 92.41(3) 3_556 . ?
C34 S34 Cu 111.34(10) . . ?
C24 S24 Cu 113.52(10) . 3_556 ?
C24 S24 Cu 105.94(10) . . ?
Cu S24 Cu 87.59(3) 3_556 . ?
C14 S14 Cu 112.15(9) . . ?
C22 C23 C24 121.0(3) . . ?
C22 C23 H23 119.5 . . ?
C24 C23 H23 119.5 . . ?
C13 C14 C15 115.6(3) . . ?
C13 C14 S14 123.7(2) . . ?
C15 C14 S14 120.8(2) . . ?
C12 C13 C14 121.4(3) . . ?
C12 C13 H13 119.3 . . ?
C14 C13 H13 119.3 . . ?
N31 C32 C33 120.9(3) . . ?
N31 C32 H32 119.5 . . ?
C33 C32 H32 119.5 . . ?
C23 C24 C25 115.9(2) . . ?
C23 C24 S24 122.7(2) . . ?
C25 C24 S24 121.4(2) . . ?
C16 N11 C12 121.0(3) . . ?
C16 N11 H11 119.5 . . ?
C12 N11 H11 119.5 . . ?
N21 C22 C23 120.2(3) . . ?
N21 C22 H22 119.9 . . ?
C23 C22 H22 119.9 . . ?
C32 C33 C34 121.1(3) . . ?
C32 C33 H33 119.5 . . ?
C34 C33 H33 119.5 . . ?
C33 C34 C35 115.2(2) . . ?
C33 C34 S34 123.4(2) . . ?
C35 C34 S34 121.3(2) . . ?
N21 C26 C25 120.9(3) . . ?
N21 C26 H26 119.6 . . ?
C25 C26 H26 119.6 . . ?
C26 N21 C22 121.1(3) . . ?
C26 N21 H21 119.5 . . ?
C22 N21 H21 119.5 . . ?
C16 C15 C14 121.3(3) . . ?
C16 C15 H15 119.4 . . ?
C14 C15 H15 119.4 . . ?
C26 C25 C24 120.8(3) . . ?
C26 C25 H25 119.6 . . ?
C24 C25 H25 119.6 . . ?
N11 C16 C15 120.4(3) . . ?
N11 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
N11 C12 C13 120.3(3) . . ?
N11 C12 H12 119.8 . . ?
C13 C12 H12 119.8 . . ?
N31 C36 C35 120.5(3) . . ?
N31 C36 H36 119.7 . . ?
C35 C36 H36 119.7 . . ?
C32 N31 C36 120.7(3) . . ?
C32 N31 H31 119.7 . . ?
C36 N31 H31 119.7 . . ?
C36 C35 C34 121.5(3) . . ?
C36 C35 H35 119.2 . . ?
C34 C35 H35 119.2 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu S14 2.2929(8) . ?
Cu S34 2.3017(8) . ?
Cu S24 2.3662(8) 3_556 ?
Cu S24 2.4329(8) . ?
S34 C34 1.712(3) . ?
S24 C24 1.719(3) . ?
S14 C14 1.708(3) . ?
C23 C22 1.356(4) . ?
C23 C24 1.409(4) . ?
C23 H23 0.9500 . ?
C14 C13 1.403(4) . ?
C14 C15 1.411(4) . ?
C13 C12 1.352(4) . ?
C13 H13 0.9500 . ?
C32 N31 1.342(3) . ?
C32 C33 1.358(4) . ?
C32 H32 0.9500 . ?
C24 C25 1.408(4) . ?
N11 C16 1.342(4) . ?
N11 C12 1.348(3) . ?
N11 H11 0.8800 . ?
C22 N21 1.345(3) . ?
C22 H22 0.9500 . ?
C33 C34 1.413(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.417(4) . ?
C26 N21 1.337(3) . ?
C26 C25 1.352(4) . ?
C26 H26 0.9500 . ?
N21 H21 0.8800 . ?
C15 C16 1.353(4) . ?
C15 H15 0.9500 . ?
C25 H25 0.9500 . ?
C16 H16 0.9500 . ?
C12 H12 0.9500 . ?
C36 N31 1.350(4) . ?
C36 C35 1.351(4) . ?
C36 H36 0.9500 . ?
N31 H31 0.8800 . ?
C35 H35 0.9500 . ?
