#------------------------------------------------------------------------------
#$Date: 2016-03-26 22:16:14 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180497 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/66/7216602.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_7216602
loop_
_publ_author_name
'Holmes, Kathryn E.'
'Kelly, Paul F.'
'Elsegood, Mark R. J.'
_publ_section_title
;
 Structural diversity within the products of the reaction of Ph2SNH with
 copper(ii) tetrafluoroborate
;
_journal_issue                   90
_journal_name_full               CrystEngComm
_journal_page_first              545
_journal_page_last               547
_journal_paper_doi               10.1039/b209185m
_journal_volume                  4
_journal_year                    2002
_chemical_formula_sum            'C48 H44 B2 Cu F8 N4 S4'
_chemical_formula_weight         1042.27
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   'geom except NH coords freely refined'
_atom_sites_solution_primary     'Patterson Synthesis'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.414(2)
_cell_angle_beta                 100.311(2)
_cell_angle_gamma                107.168(2)
_cell_formula_units_Z            1
_cell_length_a                   9.5206(7)
_cell_length_b                   10.6097(7)
_cell_length_c                   13.0115(9)
_cell_measurement_reflns_used    6808
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.99
_cell_measurement_theta_min      2.27
_cell_volume                     1184.26(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.876
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0121
_diffrn_reflns_av_sigmaI/netI    0.0206
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10615
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.99
_diffrn_reflns_theta_min         1.66
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.709
_exptl_absorpt_correction_T_max  0.866
_exptl_absorpt_correction_T_min  0.780
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             535
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.702
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         5510
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0332
_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)+(0.0376P)²+0.8423P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0811
_refine_ls_wR_factor_ref         0.0858
_reflns_number_gt                4819
_reflns_number_total             5510
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b209185m.txt
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7216602
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Cu1 Cu 0.5000 0.5000 0.5000 0.01896(8) Uani 1 2 d S
N1 N 0.58925(17) 0.66704(15) 0.62746(12) 0.0237(3) Uani 1 1 d .
H1A H 0.534(3) 0.677(2) 0.667(2) 0.036 Uiso 1 1 d .
S1 S 0.76160(5) 0.70847(4) 0.69708(3) 0.02012(10) Uani 1 1 d .
C1 C 0.82243(19) 0.87982(17) 0.78593(13) 0.0206(3) Uani 1 1 d .
C2 C 0.9790(2) 0.94925(18) 0.82052(15) 0.0247(4) Uani 1 1 d .
H2 H 1.0467 0.9082 0.7942 0.030 Uiso 1 1 calc R
C3 C 1.0346(2) 1.07942(19) 0.89415(15) 0.0275(4) Uani 1 1 d .
H3 H 1.1411 1.1286 0.9178 0.033 Uiso 1 1 calc R
C4 C 0.9356(2) 1.13831(18) 0.93354(15) 0.0274(4) Uani 1 1 d .
H4 H 0.9746 1.2269 0.9849 0.033 Uiso 1 1 calc R
C5 C 0.7795(2) 1.06792(19) 0.89792(16) 0.0305(4) Uani 1 1 d .
H5 H 0.7120 1.1085 0.9252 0.037 Uiso 1 1 calc R
C6 C 0.7214(2) 0.93835(19) 0.82257(16) 0.0278(4) Uani 1 1 d .
H6 H 0.6147 0.8908 0.7967 0.033 Uiso 1 1 calc R
C7 C 0.77034(19) 0.61667(17) 0.79740(14) 0.0217(3) Uani 1 1 d .
C8 C 0.8582(2) 0.53281(18) 0.78866(15) 0.0267(4) Uani 1 1 d .
H8 H 0.9098 0.5270 0.7327 0.032 Uiso 1 1 calc R
C9 C 0.8694(2) 0.4575(2) 0.86313(16) 0.0333(4) Uani 1 1 d .
H9 H 0.9290 0.3997 0.8582 0.040 Uiso 1 1 calc R
C10 C 0.7941(2) 0.4666(2) 0.94429(16) 0.0333(4) Uani 1 1 d .
H10 H 0.8020 0.4151 0.9950 0.040 Uiso 1 1 calc R
C11 C 0.7064(2) 0.5512(2) 0.95210(16) 0.0309(4) Uani 1 1 d .
H11 H 0.6552 0.5571 1.0083 0.037 Uiso 1 1 calc R
C12 C 0.6934(2) 0.62657(19) 0.87836(15) 0.0263(4) Uani 1 1 d .
H12 H 0.6331 0.6838 0.8831 0.032 Uiso 1 1 calc R
N2 N 0.33757(19) 0.42822(15) 0.57055(13) 0.0274(3) Uani 1 1 d .
H2A H 0.333(3) 0.471(3) 0.625(2) 0.041 Uiso 1 1 d .
S2 S 0.24093(5) 0.26887(4) 0.54936(3) 0.02293(10) Uani 1 1 d .
C13 C 0.3095(2) 0.20297(17) 0.65562(14) 0.0236(3) Uani 1 1 d .
C14 C 0.3799(2) 0.28476(19) 0.76153(15) 0.0301(4) Uani 1 1 d .
H14 H 0.3975 0.3807 0.7802 0.036 Uiso 1 1 calc R
C15 C 0.4242(2) 0.2240(2) 0.84006(16) 0.0323(4) Uani 1 1 d .
H15 H 0.4734 0.2790 0.9130 0.039 Uiso 1 1 calc R
C16 C 0.3976(2) 0.0840(2) 0.81308(17) 0.0332(4) Uani 1 1 d .
H16 H 0.4267 0.0432 0.8677 0.040 Uiso 1 1 calc R
C17 C 0.3288(3) 0.0035(2) 0.70681(19) 0.0438(5) Uani 1 1 d .
H17 H 0.3111 -0.0925 0.6883 0.053 Uiso 1 1 calc R
C18 C 0.2857(3) 0.0630(2) 0.62721(17) 0.0383(5) Uani 1 1 d .
H18 H 0.2401 0.0084 0.5537 0.046 Uiso 1 1 calc R
C19 C 0.0565(2) 0.26137(17) 0.56961(14) 0.0239(3) Uani 1 1 d .
C20 C -0.0084(2) 0.1947(2) 0.63991(15) 0.0297(4) Uani 1 1 d .
H20 H 0.0469 0.1551 0.6836 0.036 Uiso 1 1 calc R
C21 C -0.1550(2) 0.1869(2) 0.64528(17) 0.0351(4) Uani 1 1 d .
H21 H -0.2004 0.1415 0.6928 0.042 Uiso 1 1 calc R
C22 C -0.2356(2) 0.2450(2) 0.58180(17) 0.0364(5) Uani 1 1 d .
H22 H -0.3358 0.2393 0.5860 0.044 Uiso 1 1 calc R
C23 C -0.1699(2) 0.3114(2) 0.51214(17) 0.0356(4) Uani 1 1 d .
H23 H -0.2250 0.3517 0.4690 0.043 Uiso 1 1 calc R
C24 C -0.0243(2) 0.31918(19) 0.50534(16) 0.0307(4) Uani 1 1 d .
H24 H 0.0202 0.3637 0.4571 0.037 Uiso 1 1 calc R
B1 B 0.2928(3) 0.6853(2) 0.82087(19) 0.0310(5) Uani 1 1 d .
F1 F 0.4049(2) 0.7570(2) 0.91646(13) 0.0841(6) Uani 1 1 d .
F2 F 0.2431(3) 0.54595(16) 0.80834(17) 0.0802(6) Uani 1 1 d .
F3 F 0.17689(17) 0.73414(16) 0.82138(17) 0.0683(5) Uani 1 1 d .
F4 F 0.35676(15) 0.70841(14) 0.73524(10) 0.0412(3) 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'
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_1
_geom_angle_site_symmetry_3
N2 Cu1 N2 180.0 . 2_666
N2 Cu1 N1 88.55(6) . .
N2 Cu1 N1 91.45(6) 2_666 .
N2 Cu1 N1 91.45(6) . 2_666
N2 Cu1 N1 88.55(6) 2_666 2_666
N1 Cu1 N1 180.0 . 2_666
S1 N1 Cu1 119.67(9) . .
N1 S1 C1 109.16(8) . .
N1 S1 C7 110.78(8) . .
C1 S1 C7 99.17(8) . .
C6 C1 C2 121.56(16) . .
C6 C1 S1 122.64(13) . .
C2 C1 S1 115.73(13) . .
C3 C2 C1 118.83(17) . .
C4 C3 C2 120.44(17) . .
C3 C4 C5 120.06(17) . .
C4 C5 C6 120.34(17) . .
C1 C6 C5 118.74(17) . .
C12 C7 C8 121.61(17) . .
C12 C7 S1 122.66(14) . .
C8 C7 S1 115.72(13) . .
C7 C8 C9 119.03(18) . .
C10 C9 C8 120.04(18) . .
C9 C10 C11 120.32(18) . .
C12 C11 C10 120.45(18) . .
C11 C12 C7 118.55(18) . .
S2 N2 Cu1 125.43(9) . .
N2 S2 C13 111.66(9) . .
N2 S2 C19 106.63(8) . .
C13 S2 C19 100.87(8) . .
C14 C13 C18 121.01(17) . .
C14 C13 S2 122.56(14) . .
C18 C13 S2 116.41(14) . .
C13 C14 C15 118.77(18) . .
C16 C15 C14 120.65(18) . .
C17 C16 C15 120.10(19) . .
C16 C17 C18 119.92(19) . .
C17 C18 C13 119.52(19) . .
C24 C19 C20 120.60(18) . .
C24 C19 S2 116.15(14) . .
C20 C19 S2 123.12(14) . .
C21 C20 C19 119.09(18) . .
C22 C21 C20 120.49(19) . .
C21 C22 C23 120.0(2) . .
C24 C23 C22 120.16(19) . .
C23 C24 C19 119.65(18) . .
F3 B1 F2 111.0(2) . .
F3 B1 F1 108.3(2) . .
F2 B1 F1 111.7(2) . .
F3 B1 F4 110.61(19) . .
F2 B1 F4 107.95(17) . .
F1 B1 F4 107.20(19) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N2 1.9818(16) .
Cu1 N2 1.9818(16) 2_666
Cu1 N1 1.9890(15) .
Cu1 N1 1.9890(14) 2_666
N1 S1 1.6053(15) .
S1 C1 1.7922(17) .
S1 C7 1.7930(18) .
C1 C6 1.388(2) .
C1 C2 1.392(2) .
C2 C3 1.387(3) .
C3 C4 1.387(3) .
C4 C5 1.390(3) .
C5 C6 1.391(3) .
C7 C12 1.390(2) .
C7 C8 1.391(3) .
C8 C9 1.391(3) .
C9 C10 1.381(3) .
C10 C11 1.395(3) .
C11 C12 1.386(3) .
N2 S2 1.6035(15) .
S2 C13 1.7858(18) .
S2 C19 1.8034(19) .
C13 C14 1.383(2) .
C13 C18 1.388(3) .
C14 C15 1.389(3) .
C15 C16 1.384(3) .
C16 C17 1.381(3) .
C17 C18 1.386(3) .
C19 C24 1.391(3) .
C19 C20 1.393(2) .
C20 C21 1.389(3) .
C21 C22 1.386(3) .
C22 C23 1.388(3) .
C23 C24 1.384(3) .
B1 F3 1.351(3) .
B1 F2 1.375(3) .
B1 F1 1.380(3) .
B1 F4 1.395(2) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H1A F4 0.81(2) 2.12(2) 2.912(2) 165(2)
N2 H2A F4 0.78(3) 2.53(3) 3.204(2) 145(2)
