#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:16:27 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179369 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/66/4326641.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_4326641
loop_
_publ_author_name
'Irene Bassanetti'
'Luciano Marchiò'
_publ_contact_author_address
;
Departimento di Chimica GIAF
Università di Parma
via Usberti 17/a, 43100, Parma, Italy
;
_publ_contact_author_email       marchio@unipr.it
_publ_contact_author_fax         '0039 0521 905557'
_publ_contact_author_name        'Dr. Luciano Marchiò'
_publ_contact_author_phone       '0039 0521 905419'
_publ_section_title
;
 Structural Variability in Ag(I) and Cu(I) Coordination Polymers with
 Thioether-Functionalized Bis(pyrazolyl)methane Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10786
_journal_page_last               10797
_journal_paper_doi               10.1021/ic201338w
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C14 H14 Cu N4 S 1+, B F4 1-'
_chemical_formula_sum            'C14 H14 B Cu F4 N4 S'
_chemical_formula_weight         420.70
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.500(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.056(1)
_cell_length_b                   17.253(1)
_cell_length_c                   11.107(1)
_cell_measurement_reflns_used    13619
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.36
_cell_measurement_theta_min      2.21
_cell_volume                     1700.6(3)
_computing_cell_refinement       Saint
_computing_data_collection       Smart
_computing_data_reduction        Saint
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    Sir2004
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Smart APEXII CCD'
_diffrn_measurement_method       'theta & omega scan'
_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  0.0427
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            23635
_diffrn_reflns_theta_full        28.36
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         2.21
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.452
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_description       block
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         4246
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0454P)²+0.4634P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0964
_reflns_number_gt                2929
_reflns_number_total             4246
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201338w_si_001_10.cif
_cod_data_source_block           nz14
_cod_database_code               4326641
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.39616(4) 0.170250(19) 0.48131(3) 0.05170(12) Uani 1 1 d . . .
S13 S 0.31893(7) 0.23076(4) 0.07298(5) 0.04550(16) Uani 1 1 d . . .
N11 N 0.5338(2) 0.07488(11) 0.32189(16) 0.0404(4) Uani 1 1 d . . .
N21 N 0.5510(2) 0.10205(12) 0.43897(17) 0.0455(5) Uani 1 1 d . . .
C33 C 0.1766(3) 0.27212(14) 0.1441(2) 0.0444(5) Uani 1 1 d . . .
N12 N 0.2700(2) 0.09544(11) 0.24662(16) 0.0398(4) Uani 1 1 d . . .
C23 C 0.4550(3) 0.19160(13) 0.2005(2) 0.0428(5) Uani 1 1 d . . .
H23A H 0.5554 0.1957 0.1829 0.051 Uiso 1 1 calc R . .
H23B H 0.4526 0.2215 0.2740 0.051 Uiso 1 1 calc R . .
N22 N 0.2272(2) 0.13156(12) 0.34280(17) 0.0437(5) Uani 1 1 d . . .
C13 C 0.4205(2) 0.10641(13) 0.22298(19) 0.0392(5) Uani 1 1 d . . .
H13 H 0.4265 0.0775 0.1481 0.047 Uiso 1 1 calc R . .
C43 C 0.2122(3) 0.32580(15) 0.2377(2) 0.0560(7) Uani 1 1 d . . .
H43 H 0.3118 0.3406 0.2662 0.067 Uiso 1 1 calc R . .
C31 C 0.6395(3) 0.02184(15) 0.3124(2) 0.0514(6) Uani 1 1 d . . .
H31 H 0.6503 -0.0044 0.2415 0.062 Uiso 1 1 calc R . .
C11 C 0.6689(3) 0.06338(17) 0.5016(2) 0.0567(7) Uani 1 1 d . . .
H11 H 0.7065 0.0692 0.5853 0.068 Uiso 1 1 calc R . .
C32 C 0.1532(3) 0.05815(15) 0.1770(2) 0.0549(7) Uani 1 1 d . . .
H32 H 0.1555 0.0296 0.1063 0.066 Uiso 1 1 calc R . .
C22 C 0.0311(3) 0.06979(17) 0.2288(3) 0.0643(8) Uani 1 1 d . . .
H22 H -0.0661 0.0512 0.2012 0.077 Uiso 1 1 calc R . .
C12 C 0.0820(3) 0.11518(16) 0.3313(3) 0.0546(6) Uani 1 1 d . . .
H12 H 0.0222 0.1320 0.3852 0.066 Uiso 1 1 calc R . .
C83 C 0.0299(3) 0.25131(17) 0.0991(3) 0.0596(7) Uani 1 1 d . . .
H83 H 0.0067 0.2155 0.0355 0.072 Uiso 1 1 calc R . .
C53 C 0.0991(5) 0.3571(2) 0.2883(3) 0.0780(10) Uani 1 1 d . . .
H53 H 0.1220 0.3925 0.3524 0.094 Uiso 1 1 calc R . .
C21 C 0.7281(3) 0.01370(17) 0.4264(3) 0.0619(7) Uani 1 1 d . . .
H21 H 0.8112 -0.0187 0.4488 0.074 Uiso 1 1 calc R . .
C63 C -0.0489(5) 0.3358(2) 0.2439(4) 0.0889(12) Uani 1 1 d . . .
H63 H -0.1253 0.3569 0.2785 0.107 Uiso 1 1 calc R . .
C73 C -0.0835(4) 0.2842(2) 0.1496(4) 0.0822(10) Uani 1 1 d . . .
H73 H -0.1836 0.2710 0.1190 0.099 Uiso 1 1 calc R . .
B1 B 0.6093(17) 0.3851(10) 0.4315(13) 0.065(4) Uani 0.60 1 d PD A 1
F1 F 0.6421(16) 0.3136(6) 0.4540(14) 0.189(6) Uani 0.60 1 d P A 1
F3 F 0.6254(7) 0.4016(8) 0.3080(7) 0.104(2) Uani 0.60 1 d P A 1
F2 F 0.4847(7) 0.4139(5) 0.4481(7) 0.086(2) Uani 0.60 1 d P A 1
F4 F 0.7357(11) 0.4245(8) 0.4979(7) 0.147(5) Uani 0.60 1 d P A 1
B2 B 0.645(2) 0.3872(11) 0.4277(18) 0.054(5) Uani 0.40 1 d PD B 2
F6 F 0.601(3) 0.3108(11) 0.445(2) 0.065(5) Uani 0.20 1 d PD B 2
F5 F 0.7985(16) 0.4007(11) 0.4600(15) 0.088(4) Uani 0.20 1 d PD B 2
F8 F 0.588(3) 0.408(3) 0.312(2) 0.104(2) Uani 0.20 1 d PD B 2
F7 F 0.592(4) 0.4294(16) 0.511(3) 0.236(15) Uani 0.20 1 d PD B 2
F9 F 0.626(4) 0.3052(11) 0.419(3) 0.121(13) Uani 0.20 1 d PD C 3
F10 F 0.471(2) 0.3931(16) 0.452(2) 0.144(15) Uani 0.20 1 d PD D 3
F11 F 0.698(2) 0.4080(13) 0.5429(18) 0.114(7) Uani 0.20 1 d PD E 3
F12 F 0.643(3) 0.4246(11) 0.342(2) 0.160(14) Uani 0.20 1 d PD F 3
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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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'
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_3
N21 Cu N22 94.99(8) .
N21 Cu S13 153.77(6) 4_566
N22 Cu S13 110.19(6) 4_566
C33 S13 C23 103.95(11) .
C33 S13 Cu 102.76(8) 4_565
C23 S13 Cu 115.25(8) 4_565
C31 N11 N21 111.19(19) .
C31 N11 C13 127.09(19) .
N21 N11 C13 121.55(18) .
C11 N21 N11 104.7(2) .
C11 N21 Cu 135.55(18) .
N11 N21 Cu 119.00(14) .
C83 C33 C43 120.9(3) .
C83 C33 S13 117.8(2) .
C43 C33 S13 121.2(2) .
C32 N12 N22 110.9(2) .
C32 N12 C13 128.2(2) .
N22 N12 C13 120.54(17) .
C13 C23 S13 110.81(16) .
C13 C23 H23A 109.5 .
S13 C23 H23A 109.5 .
C13 C23 H23B 109.5 .
S13 C23 H23B 109.5 .
H23A C23 H23B 108.1 .
C12 N22 N12 105.0(2) .
C12 N22 Cu 135.88(18) .
N12 N22 Cu 116.86(14) .
N12 C13 N11 111.22(17) .
N12 C13 C23 112.59(18) .
N11 C13 C23 110.24(18) .
N12 C13 H13 107.5 .
N11 C13 H13 107.5 .
C23 C13 H13 107.5 .
C53 C43 C33 119.3(3) .
C53 C43 H43 120.3 .
C33 C43 H43 120.3 .
N11 C31 C21 107.1(2) .
N11 C31 H31 126.5 .
C21 C31 H31 126.5 .
N21 C11 C21 111.3(2) .
N21 C11 H11 124.3 .
C21 C11 H11 124.3 .
N12 C32 C22 107.4(2) .
N12 C32 H32 126.3 .
C22 C32 H32 126.3 .
C32 C22 C12 105.5(2) .
C32 C22 H22 127.3 .
C12 C22 H22 127.3 .
N22 C12 C22 111.2(3) .
N22 C12 H12 124.4 .
C22 C12 H12 124.4 .
C33 C83 C73 119.2(3) .
C33 C83 H83 120.4 .
C73 C83 H83 120.4 .
C43 C53 C63 119.9(3) .
C43 C53 H53 120.0 .
C63 C53 H53 120.0 .
C31 C21 C11 105.7(2) .
C31 C21 H21 127.2 .
C11 C21 H21 127.2 .
C73 C63 C53 120.4(3) .
C73 C63 H63 119.8 .
C53 C63 H63 119.8 .
C63 C73 C83 120.2(3) .
C63 C73 H73 119.9 .
C83 C73 H73 119.9 .
F2 B1 F1 121.4(15) .
F2 B1 F4 112.7(12) .
F1 B1 F4 103.3(14) .
F2 B1 F3 108.8(12) .
F1 B1 F3 108.3(13) .
F4 B1 F3 100.3(11) .
F8 B2 F7 114(2) .
F8 B2 F5 112.2(18) .
F7 B2 F5 102.0(18) .
F8 B2 F6 108(2) .
F7 B2 F6 105.7(18) .
F5 B2 F6 114.7(18) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu N21 1.958(2) .
Cu N22 2.0528(19) .
Cu S13 2.1741(7) 4_566
S13 C33 1.789(2) .
S13 C23 1.813(2) .
S13 Cu 2.1741(7) 4_565
N11 C31 1.344(3) .
N11 N21 1.362(3) .
N11 C13 1.451(3) .
N21 C11 1.331(3) .
C33 C83 1.371(4) .
C33 C43 1.382(4) .
N12 C32 1.344(3) .
N12 N22 1.358(3) .
N12 C13 1.450(3) .
C23 C13 1.534(3) .
C23 H23A 0.9700 .
C23 H23B 0.9700 .
N22 C12 1.326(3) .
C13 H13 0.9800 .
C43 C53 1.374(4) .
C43 H43 0.9300 .
C31 C21 1.365(4) .
C31 H31 0.9300 .
C11 C21 1.377(4) .
C11 H11 0.9300 .
C32 C22 1.359(4) .
C32 H32 0.9300 .
C22 C12 1.383(4) .
C22 H22 0.9300 .
C12 H12 0.9300 .
C83 C73 1.386(4) .
C83 H83 0.9300 .
C53 C63 1.382(6) .
C53 H53 0.9300 .
C21 H21 0.9300 .
C63 C73 1.363(5) .
C63 H63 0.9300 .
C73 H73 0.9300 .
B1 F2 1.280(17) .
B1 F1 1.282(19) .
B1 F4 1.407(16) .
B1 F3 1.437(14) .
B2 F8 1.328(17) .
B2 F7 1.338(17) .
B2 F5 1.388(17) .
B2 F6 1.400(16) .
