#------------------------------------------------------------------------------
#$Date: 2016-03-26 22:16:14 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180497 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/66/7216601.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_7216601
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           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 except NH coords freely refined'
_atom_sites_solution_primary     'patterson synthesis'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.988(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.2158(7)
_cell_length_b                   19.9156(9)
_cell_length_c                   14.3422(6)
_cell_measurement_reflns_used    12868
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.82
_cell_measurement_theta_min      2.35
_cell_volume                     4771.6(4)
_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 1.000
_diffrn_measured_fraction_theta_max 0.905
_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  0.0135
_diffrn_reflns_av_sigmaI/netI    0.0137
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20755
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.94
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.703
_exptl_absorpt_correction_T_max  0.796
_exptl_absorpt_correction_T_min  0.654
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2140
_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         5716
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0293
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0346P)²+5.6731P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0783
_reflns_number_gt                4933
_reflns_number_total             5716
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b209185m.txt
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7216601
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Cu1 Cu 0.0000 0.815655(11) 0.7500 0.01984(7) Uani 1 2 d S
N1 N -0.01800(10) 0.75198(7) 0.64393(10) 0.0324(3) Uani 1 1 d .
H1A H -0.0432(14) 0.7611(12) 0.5882(17) 0.049 Uiso 1 1 d .
S1 S 0.02249(2) 0.679699(18) 0.64836(3) 0.02620(9) Uani 1 1 d .
C1 C -0.05481(9) 0.61929(8) 0.60353(11) 0.0261(3) Uani 1 1 d .
C2 C -0.13405(10) 0.63720(9) 0.59266(12) 0.0337(4) Uani 1 1 d .
H2 H -0.1482 0.6821 0.6036 0.040 Uiso 1 1 calc R
C3 C -0.19270(11) 0.58827(10) 0.56542(14) 0.0383(4) Uani 1 1 d .
H3 H -0.2475 0.5999 0.5570 0.046 Uiso 1 1 calc R
C4 C -0.17213(11) 0.52299(9) 0.55055(13) 0.0359(4) Uani 1 1 d .
H4 H -0.2127 0.4899 0.5318 0.043 Uiso 1 1 calc R
C5 C -0.09252(11) 0.50554(9) 0.56290(13) 0.0363(4) Uani 1 1 d .
H5 H -0.0785 0.4604 0.5530 0.044 Uiso 1 1 calc R
C6 C -0.03317(10) 0.55350(8) 0.58959(12) 0.0319(3) Uani 1 1 d .
H6 H 0.0216 0.5416 0.5983 0.038 Uiso 1 1 calc R
C7 C 0.07933(10) 0.67502(7) 0.55970(12) 0.0282(3) Uani 1 1 d .
C8 C 0.04422(11) 0.68534(8) 0.46295(12) 0.0333(4) Uani 1 1 d .
H8 H -0.0119 0.6922 0.4414 0.040 Uiso 1 1 calc R
C9 C 0.09238(14) 0.68552(9) 0.39845(15) 0.0436(4) Uani 1 1 d .
H9 H 0.0695 0.6931 0.3321 0.052 Uiso 1 1 calc R
C10 C 0.17382(14) 0.67467(11) 0.43054(19) 0.0548(6) Uani 1 1 d .
H10 H 0.2065 0.6742 0.3858 0.066 Uiso 1 1 calc R
C11 C 0.20791(13) 0.66455(13) 0.5265(2) 0.0573(6) Uani 1 1 d .
H11 H 0.2639 0.6571 0.5476 0.069 Uiso 1 1 calc R
C12 C 0.16100(11) 0.66523(10) 0.59269(15) 0.0421(4) Uani 1 1 d .
H12 H 0.1844 0.6591 0.6592 0.051 Uiso 1 1 calc R
N2 N 0.06605(9) 0.88070(7) 0.83625(10) 0.0338(3) Uani 1 1 d .
H2A H 0.0925(14) 0.8709(12) 0.8905(17) 0.051 Uiso 1 1 d .
S2 S 0.09788(2) 0.948533(18) 0.80019(3) 0.02475(9) Uani 1 1 d .
C13 C 0.20353(9) 0.94114(8) 0.80805(11) 0.0274(3) Uani 1 1 d .
C14 C 0.24028(12) 0.87916(9) 0.82474(13) 0.0388(4) Uani 1 1 d .
H14 H 0.2112 0.8409 0.8369 0.047 Uiso 1 1 calc R
C15 C 0.32047(13) 0.87377(10) 0.82346(16) 0.0481(5) Uani 1 1 d .
H15 H 0.3467 0.8315 0.8352 0.058 Uiso 1 1 calc R
C16 C 0.36224(12) 0.92923(11) 0.80528(14) 0.0447(5) Uani 1 1 d .
H16 H 0.4172 0.9252 0.8054 0.054 Uiso 1 1 calc R
C17 C 0.32441(11) 0.99102(10) 0.78681(13) 0.0378(4) Uani 1 1 d .
H17 H 0.3533 1.0290 0.7734 0.045 Uiso 1 1 calc R
C18 C 0.24468(10) 0.99743(8) 0.78795(12) 0.0314(3) Uani 1 1 d .
H18 H 0.2184 1.0396 0.7752 0.038 Uiso 1 1 calc R
C19 C 0.09619(9) 1.01329(8) 0.88537(11) 0.0264(3) Uani 1 1 d .
C20 C 0.10432(11) 0.99878(11) 0.98125(13) 0.0413(4) Uani 1 1 d .
H20 H 0.1139 0.9542 1.0049 0.050 Uiso 1 1 calc R
C21 C 0.09798(14) 1.05166(15) 1.04202(16) 0.0637(7) Uani 1 1 d .
H21 H 0.1040 1.0432 1.1086 0.076 Uiso 1 1 calc R
C22 C 0.08311(13) 1.11606(14) 1.0077(2) 0.0638(7) Uani 1 1 d .
H22 H 0.0788 1.1515 1.0506 0.077 Uiso 1 1 calc R
C23 C 0.07458(12) 1.12922(11) 0.9125(2) 0.0542(6) Uani 1 1 d .
H23 H 0.0640 1.1737 0.8891 0.065 Uiso 1 1 calc R
C24 C 0.08130(11) 1.07778(9) 0.84965(15) 0.0377(4) Uani 1 1 d .
H24 H 0.0758 1.0867 0.7833 0.045 Uiso 1 1 calc R
B1 B -0.14487(12) 0.81494(10) 0.36186(14) 0.0329(4) Uani 1 1 d .
F1 F -0.09165(7) 0.77938(6) 0.32256(9) 0.0486(3) Uani 1 1 d .
F2 F -0.12570(8) 0.80597(7) 0.46150(8) 0.0570(3) Uani 1 1 d .
F3 F -0.13960(9) 0.88261(6) 0.34494(10) 0.0587(3) Uani 1 1 d .
F4 F -0.22171(7) 0.79299(8) 0.32432(10) 0.0629(4) 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
N1 Cu1 N1 98.71(8) . 2_556
N1 Cu1 N2 152.18(7) . .
N1 Cu1 N2 88.79(6) 2_556 .
N1 Cu1 N2 88.79(6) . 2_556
N1 Cu1 N2 152.19(7) 2_556 2_556
N2 Cu1 N2 96.99(9) . 2_556
S1 N1 Cu1 124.86(8) . .
N1 S1 C7 109.18(8) . .
N1 S1 C1 108.17(8) . .
C7 S1 C1 101.34(7) . .
C2 C1 C6 121.25(15) . .
C2 C1 S1 119.60(12) . .
C6 C1 S1 118.84(12) . .
C1 C2 C3 118.76(16) . .
C4 C3 C2 120.58(17) . .
C3 C4 C5 120.07(17) . .
C4 C5 C6 120.30(16) . .
C5 C6 C1 119.02(15) . .
C12 C7 C8 121.54(17) . .
C12 C7 S1 116.76(14) . .
C8 C7 S1 121.56(13) . .
C9 C8 C7 118.84(18) . .
C10 C9 C8 120.0(2) . .
C11 C10 C9 120.6(2) . .
C10 C11 C12 120.4(2) . .
C7 C12 C11 118.6(2) . .
S2 N2 Cu1 123.40(8) . .
N2 S2 C19 109.14(8) . .
N2 S2 C13 109.40(8) . .
C19 S2 C13 101.53(7) . .
C14 C13 C18 121.37(16) . .
C14 C13 S2 119.82(13) . .
C18 C13 S2 118.53(12) . .
C13 C14 C15 118.80(18) . .
C16 C15 C14 120.45(18) . .
C15 C16 C17 120.33(18) . .
C18 C17 C16 120.07(18) . .
C17 C18 C13 118.96(16) . .
C20 C19 C24 121.93(17) . .
C20 C19 S2 121.18(14) . .
C24 C19 S2 116.77(13) . .
C19 C20 C21 117.6(2) . .
C22 C21 C20 121.3(2) . .
C23 C22 C21 120.2(2) . .
C22 C23 C24 120.2(2) . .
C19 C24 C23 118.8(2) . .
F4 B1 F3 109.93(16) . .
F4 B1 F1 110.36(16) . .
F3 B1 F1 110.58(16) . .
F4 B1 F2 109.09(17) . .
F3 B1 F2 107.22(16) . .
F1 B1 F2 109.60(15) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N1 1.9469(13) .
Cu1 N1 1.9469(13) 2_556
Cu1 N2 1.9549(14) .
Cu1 N2 1.9549(14) 2_556
N1 S1 1.5940(14) .
S1 C7 1.7845(17) .
S1 C1 1.7940(16) .
C1 C2 1.382(2) .
C1 C6 1.390(2) .
C2 C3 1.390(3) .
C3 C4 1.378(3) .
C4 C5 1.383(3) .
C5 C6 1.383(2) .
C7 C12 1.385(2) .
C7 C8 1.388(2) .
C8 C9 1.383(3) .
C9 C10 1.383(3) .
C10 C11 1.375(4) .
C11 C12 1.387(3) .
N2 S2 1.5904(14) .
S2 C19 1.7815(16) .
S2 C13 1.8010(16) .
C13 C14 1.381(2) .
C13 C18 1.393(2) .
C14 C15 1.389(3) .
C15 C16 1.377(3) .
C16 C17 1.388(3) .
C17 C18 1.383(2) .
C19 C20 1.379(2) .
C19 C24 1.384(2) .
C20 C21 1.388(3) .
C21 C22 1.375(4) .
C22 C23 1.363(4) .
C23 C24 1.388(3) .
B1 F4 1.374(2) .
B1 F3 1.376(2) .
B1 F1 1.381(2) .
B1 F2 1.398(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
_geom_hbond_site_symmetry_A
N1 H1A F2 0.83(2) 2.21(2) 3.0157(18) 164(2) .
N2 H2A F2 0.82(2) 2.43(2) 3.2006(19) 155(2) 2_556
