#------------------------------------------------------------------------------
#$Date: 2016-02-16 02:10:39 +0100 (mar 16 de feb de 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/08/7010830.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_7010830
loop_
_publ_author_name
'Ball, Rachel J.'
'Genge, Anthony R. J.'
'Radford, Alison L.'
'Skelton, Brian W.'
'Tolhurst, Vicki-Anne'
'White, Allan H.'
_publ_section_title
;
 Complexes of late transition metals containing the mixed donor ligands
 2,6-(RSCH2)2C5H3N (R = Ph, Me): Crystal structures of
 [{Cu(2,6-(PhSCH2)2C5H3N)(µ-X)}2] (X = Cl, Br) and
 [Ni(2,6-(PhSCH2)2C5H3N)Br2]
;
_journal_issue                   19
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2807
_journal_paper_doi               10.1039/b104332n
_journal_year                    2001
_chemical_formula_moiety         'C38 H34 Br2 Cu2 N2 S4 '
_chemical_formula_sum            'C38 H34 Br2 Cu2 N2 S4'
_chemical_formula_weight         933.84
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2001-05-11
_audit_creation_method           'by teXsan for Windows v1.06'
_audit_update_record
;
?
;
_cell_angle_alpha                105.25(3)
_cell_angle_beta                 96.69(2)
_cell_angle_gamma                106.58(3)
_cell_formula_units_Z            1
_cell_length_a                   10.035(2)
_cell_length_b                   13.133(6)
_cell_length_c                   7.866(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293.2
_cell_measurement_theta_max      18.7
_cell_measurement_theta_min      15.9
_cell_volume                     937.8(6)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction
;
teXsan for Windows version 1.06 (MSC, 1997-1999)
;
_computing_publication_material
;
teXsan for Windows version 1.06 (MSC, 1997-1999)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
SIR92 (Altomare, et. al. 1994)
;
_diffrn_ambient_temperature      150.1
_diffrn_measurement_device_type  'Rigaku AFC7S'
_diffrn_measurement_method       ω-2θ
_diffrn_orient_matrix_UB_11      -0.00525
_diffrn_orient_matrix_UB_12      0.05216
_diffrn_orient_matrix_UB_13      0.11534
_diffrn_orient_matrix_UB_21      -0.03708
_diffrn_orient_matrix_UB_22      0.04375
_diffrn_orient_matrix_UB_23      -0.06879
_diffrn_orient_matrix_UB_31      -0.09946
_diffrn_orient_matrix_UB_32      -0.04852
_diffrn_orient_matrix_UB_33      -0.01026
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.02650
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3506
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        0.69
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.517
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.610
_exptl_absorpt_correction_type
;
psi-scans (North,Phillips & Matthews, 1968)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             468.00
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3302
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0508
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1456
_refine_ls_wR_factor_ref         0.1616
_reflns_number_gt                2296
_reflns_number_total             3302
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b104332n.txt
_cod_data_source_block           '_rb06_CuBrS2N'
_cod_original_cell_volume        937.8(7)
_cod_original_sg_symbol_H-M      'P -1       '
_cod_original_formula_sum        'C38 H34 Br2 Cu2 N2 S4 '
_cod_database_code               7010830
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.59116(6) 0.49122(5) 0.77768(8) 0.0506(2) Uani 1 d . . .
Cu1 Cu 0.37273(7) 0.45168(7) 0.88056(10) 0.0569(3) Uani 1 d . . .
S1 S 0.20753(16) 0.26639(12) 0.78468(19) 0.0493(4) Uani 1 d . . .
S2 S 0.3855(3) 0.81436(17) 0.8340(3) 0.0854(6) Uani 1 d . . .
N1 N 0.2008(4) 0.4984(4) 0.8004(6) 0.0430(10) Uani 1 d . . .
C1 C 0.0683(6) 0.3234(5) 0.8468(8) 0.0543(15) Uani 1 d . . .
C2 C 0.3538(7) 0.6668(5) 0.7627(10) 0.0644(17) Uani 1 d . . .
C3 C 0.2080(6) 0.5929(5) 0.7635(8) 0.0487(14) Uani 1 d . . .
C4 C 0.0850(7) 0.6182(6) 0.7158(8) 0.0605(16) Uani 1 d . . .
C5 C -0.0458(7) 0.5443(6) 0.7095(9) 0.0635(17) Uani 1 d . . .
C6 C -0.0524(6) 0.4486(6) 0.7498(8) 0.0580(17) Uani 1 d . . .
C7 C 0.0730(5) 0.4265(5) 0.7941(7) 0.0436(13) Uani 1 d . . .
C11 C 0.1552(6) 0.2193(5) 0.5459(7) 0.0465(13) Uani 1 d . . .
C12 C 0.0272(6) 0.1352(5) 0.4637(8) 0.0564(15) Uani 1 d . . .
C13 C -0.0107(7) 0.0988(6) 0.2773(9) 0.0687(19) Uani 1 d . . .
C14 C 0.0762(8) 0.1417(6) 0.1722(8) 0.0625(17) Uani 1 d . . .
C15 C 0.2031(8) 0.2228(6) 0.2540(9) 0.0656(18) Uani 1 d . . .
C16 C 0.2441(6) 0.2624(5) 0.4416(8) 0.0523(14) Uani 1 d . . .
C21 C 0.3637(7) 0.8424(6) 1.0615(10) 0.0647(18) Uani 1 d . . .
C22 C 0.3150(8) 0.9337(7) 1.1270(12) 0.082(2) Uani 1 d . . .
C23 C 0.3017(9) 0.9615(7) 1.3023(13) 0.081(2) Uani 1 d . . .
C24 C 0.3335(9) 0.9050(8) 1.4139(11) 0.086(2) Uani 1 d . . .
C25 C 0.3780(9) 0.8155(8) 1.3488(13) 0.089(2) Uani 1 d . . .
C26 C 0.3942(10) 0.7881(7) 1.1747(13) 0.085(2) Uani 1 d . . .
H1A H -0.0211 0.2676 0.7895 0.065 Uiso 1 d . . .
H1B H 0.0778 0.3419 0.9738 0.065 Uiso 1 d . . .
H2A H 0.3687 0.6463 0.6431 0.077 Uiso 1 d . . .
H2B H 0.4212 0.6524 0.8402 0.077 Uiso 1 d . . .
H4 H 0.0917 0.6855 0.6881 0.072 Uiso 1 d . . .
H5 H -0.1303 0.5600 0.6773 0.076 Uiso 1 d . . .
H6 H -0.1415 0.3972 0.7480 0.070 Uiso 1 d . . .
H12 H -0.0338 0.1033 0.5334 0.068 Uiso 1 d . . .
H13 H -0.0995 0.0421 0.2202 0.082 Uiso 1 d . . .
H14 H 0.0479 0.1150 0.0446 0.075 Uiso 1 d . . .
H15 H 0.2643 0.2529 0.1832 0.078 Uiso 1 d . . .
H16 H 0.3334 0.3188 0.4978 0.063 Uiso 1 d . . .
H22 H 0.2918 0.9742 1.0500 0.098 Uiso 1 d . . .
H23 H 0.2694 1.0227 1.3477 0.098 Uiso 1 d . . .
H24 H 0.3249 0.9271 1.5360 0.103 Uiso 1 d . . .
H25 H 0.3969 0.7732 1.4239 0.107 Uiso 1 d . . .
H26 H 0.4292 0.7281 1.1317 0.102 Uiso 1 d . . .
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0 38 0.002 0.002
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
H 0 34 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
N 0 2 0.004 0.003
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
S 0 4 0.110 0.124
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
Cu 0 2 0.263 1.266
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Br 0 2 -0.374 2.456
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
-4 0 1
-4 1 1
-4 3 0
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
Cu1 Br1 Cu1 67.03(4) . 2_667 ?
N1 Cu1 S1 85.59(14) . . ?
N1 Cu1 Br1 125.29(13) . . ?
S1 Cu1 Br1 120.58(6) . . ?
N1 Cu1 Br1 104.23(12) . 2_667 ?
S1 Cu1 Br1 103.59(6) . 2_667 ?
Br1 Cu1 Br1 112.97(4) . 2_667 ?
N1 Cu1 Cu1 137.35(13) . 2_667 ?
S1 Cu1 Cu1 131.68(7) . 2_667 ?
Br1 Cu1 Cu1 59.20(4) . 2_667 ?
Br1 Cu1 Cu1 53.78(4) 2_667 2_667 ?
C11 S1 C1 100.8(3) . . ?
C11 S1 Cu1 109.3(2) . . ?
C1 S1 Cu1 89.2(2) . . ?
C21 S2 C2 103.0(3) . . ?
C3 N1 C7 119.2(5) . . ?
C3 N1 Cu1 125.8(4) . . ?
C7 N1 Cu1 114.9(4) . . ?
C7 C1 S1 113.9(4) . . ?
C7 C1 H1A 108.4(6) . . ?
S1 C1 H1A 108.4(5) . . ?
C7 C1 H1B 108.3(5) . . ?
S1 C1 H1B 108.3(5) . . ?
H1A C1 H1B 109.5(6) . . ?
C3 C2 S2 116.6(5) . . ?
C3 C2 H2A 107.7(6) . . ?
S2 C2 H2A 107.7(5) . . ?
C3 C2 H2B 107.6(6) . . ?
S2 C2 H2B 107.7(6) . . ?
H2A C2 H2B 109.4(6) . . ?
N1 C3 C4 121.3(5) . . ?
N1 C3 C2 116.6(5) . . ?
C4 C3 C2 121.9(6) . . ?
C5 C4 C3 119.2(6) . . ?
C5 C4 H4 120.3(6) . . ?
C3 C4 H4 120.4(7) . . ?
C6 C5 C4 119.2(6) . . ?
C6 C5 H5 120.4(7) . . ?
C4 C5 H5 120.4(8) . . ?
C5 C6 C7 119.4(6) . . ?
C5 C6 H6 120.4(7) . . ?
C7 C6 H6 120.2(7) . . ?
N1 C7 C6 121.6(6) . . ?
N1 C7 C1 118.1(5) . . ?
C6 C7 C1 120.2(5) . . ?
C12 C11 C16 119.8(5) . . ?
C12 C11 S1 119.5(5) . . ?
C16 C11 S1 120.7(4) . . ?
C11 C12 C13 118.5(6) . . ?
C11 C12 H12 120.8(6) . . ?
C13 C12 H12 120.7(6) . . ?
C14 C13 C12 122.2(6) . . ?
C14 C13 H13 118.9(7) . . ?
C12 C13 H13 118.8(7) . . ?
C15 C14 C13 118.9(6) . . ?
C15 C14 H14 120.6(7) . . ?
C13 C14 H14 120.6(7) . . ?
C14 C15 C16 120.5(6) . . ?
C14 C15 H15 119.8(7) . . ?
C16 C15 H15 119.8(7) . . ?
C11 C16 C15 120.1(5) . . ?
C11 C16 H16 119.9(6) . . ?
C15 C16 H16 120.0(6) . . ?
C26 C21 C22 118.4(8) . . ?
C26 C21 S2 125.8(7) . . ?
C22 C21 S2 115.7(6) . . ?
C23 C22 C21 118.1(7) . . ?
C23 C22 H22 121.1(9) . . ?
C21 C22 H22 120.8(9) . . ?
C24 C23 C22 122.1(8) . . ?
C24 C23 H23 119.0(9) . . ?
C22 C23 H23 118.8(9) . . ?
C23 C24 C25 119.4(8) . . ?
C23 C24 H24 120.3(10) . . ?
C25 C24 H24 120.3(10) . . ?
C26 C25 C24 118.9(8) . . ?
C26 C25 H25 120.6(10) . . ?
C24 C25 H25 120.4(10) . . ?
C21 C26 C25 122.9(8) . . ?
C21 C26 H26 118.4(9) . . ?
C25 C26 H26 118.7(9) . . ?
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
Br1 Cu1 2.3905(11) . ?
Br1 Cu1 2.5453(12) 2_667 ?
Cu1 N1 2.074(4) . ?
Cu1 S1 2.383(2) . ?
Cu1 Br1 2.5453(12) 2_667 ?
Cu1 Cu1 2.7282(18) 2_667 ?
S1 C11 1.778(6) . ?
S1 C1 1.820(6) . ?
S2 C21 1.783(8) . ?
S2 C2 1.790(7) . ?
N1 C3 1.332(7) . ?
N1 C7 1.345(7) . ?
C1 C7 1.508(9) . ?
C1 H1A 0.950(6) . ?
C1 H1B 0.950(6) . ?
C2 C3 1.509(8) . ?
C2 H2A 0.950(7) . ?
C2 H2B 0.950(7) . ?
C3 C4 1.402(8) . ?
C4 C5 1.378(10) . ?
C4 H4 0.951(7) . ?
C5 C6 1.361(10) . ?
C5 H5 0.950(6) . ?
C6 C7 1.395(8) . ?
C6 H6 0.950(6) . ?
C11 C12 1.381(8) . ?
C11 C16 1.384(8) . ?
C12 C13 1.386(9) . ?
C12 H12 0.951(6) . ?
C13 C14 1.376(10) . ?
C13 H13 0.950(6) . ?
C14 C15 1.359(10) . ?
C14 H14 0.950(6) . ?
C15 C16 1.396(9) . ?
C15 H15 0.950(7) . ?
C16 H16 0.951(6) . ?
C21 C26 1.337(11) . ?
C21 C22 1.418(11) . ?
C22 C23 1.364(12) . ?
C22 H22 0.954(8) . ?
C23 C24 1.355(12) . ?
C23 H23 0.950(8) . ?
C24 C25 1.372(12) . ?
C24 H24 0.949(9) . ?
C25 C26 1.364(13) . ?
C25 H25 0.948(9) . ?
C26 H26 0.951(8) . ?
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
C(1) C(5) 3.54(1) . 2_567 no
C(4) C(5) 3.37(1) . 2_566 no
C(4) C(6) 3.46(1) . 2_566 no
C(5) C(5) 3.51(2) . 2_566 no
C(6) C(7) 3.60(1) . 2_567 no
C(12) C(12) 3.60(2) . 2_556 no
C(24) C(24) 3.40(3) . 2_678 no
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
? ? ? ? ? ? ? ? ? ?
