#------------------------------------------------------------------------------
#$Date: 2015-10-09 13:25:49 +0300 (Fri, 09 Oct 2015) $
#$Revision: 161627 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/61/7036195.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_7036195
loop_
_publ_author_name
'Kimani, Martin M.'
'Watts, David'
'Graham, Leigh A.'
'Rabinovich, Daniel'
'Yap, Glenn P. A.'
'Brumaghim, Julia L.'
_publ_section_title
;
 Dinuclear copper(i) complexes with N-heterocyclic thione and selone
 ligands: synthesis, characterization, and electrochemical studies.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16313
_journal_page_last               16324
_journal_paper_doi               10.1039/c5dt02232k
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C30 H42 Cu2 N12 S6''2 (B F4)'
_chemical_formula_sum            'C30 H42 B2 Cu2 F8 N12 S6'
_chemical_formula_weight         1063.82
_chemical_name_systematic        '[Cu2(BmeMe)3](BF4)2'
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_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_method           SHELXL-97
_audit_update_record
;
2015-06-08 deposited with the CCDC.
2015-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                98.29(3)
_cell_angle_beta                 116.81(3)
_cell_angle_gamma                91.25(3)
_cell_formula_units_Z            1
_cell_length_a                   10.370(2)
_cell_length_b                   10.700(2)
_cell_length_c                   10.810(2)
_cell_measurement_reflns_used    9129
_cell_measurement_temperature    168.15
_cell_measurement_theta_max      26.29
_cell_measurement_theta_min      3.08
_cell_volume                     1054.2(5)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC,2006)'
_computing_data_collection       'CrystalClear (Rigaku/MSC,2006)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC,2006)'
_computing_molecular_graphics    'SHELXTL 6.10 (Sheldrick,2008)'
_computing_publication_material  'SHELXTL 6.10 (Sheldrick,2008)'
_computing_structure_refinement  'SHELXTL 6.10 (Sheldrick,2008)'
_computing_structure_solution    'SHELXTL 6.10 (Sheldrick,2008)'
_diffrn_ambient_temperature      168.15
_diffrn_detector_area_resol_mean 14.6306
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Rigaku AFC8S'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_sigmaI/netI    0.0523
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9129
_diffrn_reflns_theta_full        26.29
_diffrn_reflns_theta_max         26.29
_diffrn_reflns_theta_min         3.08
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.383
_exptl_absorpt_correction_T_max  0.7506
_exptl_absorpt_correction_T_min  0.6737
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB, CrystalClear'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             542
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile/diethyl ether'
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.925
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         4210
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0769P)²+1.6712P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1349
_refine_ls_wR_factor_ref         0.1564
_reflns_number_gt                3066
_reflns_number_total             4210
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt02232k2.cif
_cod_data_source_block           cuebit
_cod_depositor_comments
'Adding full bibliography for 7036192--7036198.cif.'
_cod_original_cell_volume        1054.2(4)
_cod_database_code               7036195
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 0.00438(7) 0.41483(6) 0.14069(6) 0.0381(2) Uani 1 1 d .
S2 S 0.17730(13) 0.49073(11) 0.02094(12) 0.0292(3) Uani 1 1 d .
S1 S -0.01125(13) 0.19639(10) 0.10415(12) 0.0308(3) Uani 1 1 d .
S3 S 0.13921(12) 0.51060(10) 0.37019(12) 0.0284(3) Uani 1 1 d .
N5 N 0.3639(4) 0.3600(4) 0.4392(4) 0.0264(8) Uani 1 1 d .
N2 N 0.0894(4) 0.1256(3) -0.0861(4) 0.0290(8) Uani 1 1 d .
N4 N 0.3148(4) 0.4385(4) -0.1450(4) 0.0319(8) Uani 1 1 d .
N6 N 0.1804(4) 0.2778(4) 0.4559(4) 0.0285(8) Uani 1 1 d .
N3 N 0.3397(4) 0.3024(4) -0.0087(4) 0.0318(8) Uani 1 1 d .
C11 C 0.2278(5) 0.3804(4) 0.4232(4) 0.0246(8) Uani 1 1 d .
N1 N -0.1316(4) 0.1675(4) -0.1847(4) 0.0331(9) Uani 1 1 d .
C10 C 0.2762(5) 0.4101(4) -0.0483(5) 0.0265(9) Uani 1 1 d .
C1 C -0.0190(5) 0.1625(4) -0.0597(4) 0.0262(9) Uani 1 1 d .
C6 C 0.3255(5) 0.2337(4) 0.0914(5) 0.0333(10) Uani 1 1 d .
H6A H 0.2803 0.2848 0.1398 0.040 Uiso 1 1 calc R
H6B H 0.4213 0.2200 0.1612 0.040 Uiso 1 1 calc R
C12 C 0.4619(5) 0.4527(5) 0.4294(4) 0.0297(10) Uani 1 1 d .
H12A H 0.4079 0.4982 0.3532 0.036 Uiso 1 1 calc R
H12B H 0.5340 0.4100 0.4098 0.036 Uiso 1 1 calc R
C15 C 0.0377(6) 0.2568(5) 0.4501(6) 0.0397(12) Uani 1 1 d .
H15A H 0.0203 0.3299 0.5012 0.060 Uiso 1 1 calc R
H15B H 0.0351 0.1838 0.4915 0.060 Uiso 1 1 calc R
H15C H -0.0359 0.2427 0.3538 0.060 Uiso 1 1 calc R
C13 C 0.3978(5) 0.2416(5) 0.4771(5) 0.0330(10) Uani 1 1 d .
H13A H 0.4829 0.2045 0.4926 0.040 Uiso 1 1 calc R
C14 C 0.2841(6) 0.1912(5) 0.4870(5) 0.0359(11) Uani 1 1 d .
H14A H 0.2759 0.1122 0.5105 0.043 Uiso 1 1 calc R
C9 C 0.2772(6) 0.5517(5) -0.2132(6) 0.0416(12) Uani 1 1 d .
H9A H 0.2768 0.6220 -0.1473 0.062 Uiso 1 1 calc R
H9B H 0.1828 0.5345 -0.2930 0.062 Uiso 1 1 calc R
H9C H 0.3477 0.5722 -0.2437 0.062 Uiso 1 1 calc R
C4 C 0.0451(7) 0.1089(5) -0.2291(6) 0.0429(12) Uani 1 1 d .
H4A H 0.1007 0.0838 -0.2742 0.051 Uiso 1 1 calc R
C5 C 0.2354(5) 0.1064(4) 0.0213(6) 0.0361(11) Uani 1 1 d .
H5A H 0.2829 0.0528 -0.0225 0.043 Uiso 1 1 calc R
H5B H 0.2271 0.0644 0.0914 0.043 Uiso 1 1 calc R
C3 C -0.0924(7) 0.1357(5) -0.2901(5) 0.0434(13) Uani 1 1 d .
H3A H -0.1508 0.1334 -0.3859 0.052 Uiso 1 1 calc R
C2 C -0.2783(6) 0.1969(5) -0.2088(6) 0.0465(13) Uani 1 1 d .
H2A H -0.2799 0.2171 -0.1201 0.070 Uiso 1 1 calc R
H2B H -0.3467 0.1246 -0.2650 0.070 Uiso 1 1 calc R
H2C H -0.3040 0.2681 -0.2570 0.070 Uiso 1 1 calc R
C8 C 0.4020(6) 0.3516(5) -0.1660(6) 0.0417(12) Uani 1 1 d .
H8A H 0.4429 0.3522 -0.2267 0.050 Uiso 1 1 calc R
C7 C 0.4170(6) 0.2655(5) -0.0822(6) 0.0430(12) Uani 1 1 d .
H7A H 0.4690 0.1950 -0.0750 0.052 Uiso 1 1 calc R
F1 F 0.7798(3) 0.0335(3) 0.3722(3) 0.0394(7) Uani 1 1 d .
F2 F 0.6607(5) 0.2101(4) 0.3541(5) 0.0796(14) Uani 1 1 d .
B1 B 0.6493(6) 0.0861(5) 0.3026(6) 0.0326(11) Uani 1 1 d .
F4 F 0.5493(6) 0.0294(6) 0.3257(11) 0.173(4) Uani 1 1 d .
F3 F 0.6091(9) 0.0682(8) 0.1682(5) 0.179(5) 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
S3 Cu1 S2 122.49(5) . 2_565
S3 Cu1 S1 114.70(6) . .
S2 Cu1 S1 117.71(6) 2_565 .
S3 Cu1 S2 101.01(5) . .
S2 Cu1 S2 86.40(5) 2_565 .
S1 Cu1 S2 105.69(5) . .
C10 S2 Cu1 112.45(16) . 2_565
C10 S2 Cu1 132.88(16) . .
Cu1 S2 Cu1 93.60(5) 2_565 .
C1 S1 Cu1 101.55(15) . .
C11 S3 Cu1 94.78(15) . .
C11 N5 C13 109.6(4) . .
C11 N5 C12 124.8(4) . .
C13 N5 C12 125.4(4) . .
C1 N2 C4 109.8(4) . .
C1 N2 C5 125.1(4) . .
C4 N2 C5 125.0(4) . .
C10 N4 C8 110.8(4) . .
C10 N4 C9 125.0(4) . .
C8 N4 C9 124.2(4) . .
C11 N6 C14 109.5(4) . .
C11 N6 C15 125.2(4) . .
C14 N6 C15 125.1(4) . .
C10 N3 C7 109.8(4) . .
C10 N3 C6 125.5(4) . .
C7 N3 C6 124.7(4) . .
N6 C11 N5 106.1(4) . .
N6 C11 S3 128.4(3) . .
N5 C11 S3 125.6(3) . .
C1 N1 C3 109.9(4) . .
C1 N1 C2 125.9(4) . .
C3 N1 C2 124.2(4) . .
N4 C10 N3 105.3(4) . .
N4 C10 S2 129.4(4) . .
N3 C10 S2 125.2(3) . .
N2 C1 N1 106.3(4) . .
N2 C1 S1 125.7(3) . .
N1 C1 S1 128.0(4) . .
N3 C6 C5 112.3(4) . .
N5 C12 C12 109.2(4) . 2_666
C14 C13 N5 106.7(4) . .
C13 C14 N6 108.0(4) . .
C3 C4 N2 107.0(5) . .
N2 C5 C6 109.9(4) . .
C4 C3 N1 107.0(5) . .
C7 C8 N4 107.3(4) . .
C8 C7 N3 106.8(5) . .
F3 B1 F4 109.6(8) . .
F3 B1 F2 110.9(6) . .
F4 B1 F2 106.6(6) . .
F3 B1 F1 109.9(5) . .
F4 B1 F1 108.4(5) . .
F2 B1 F1 111.4(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 S3 2.2880(16) .
Cu1 S2 2.2905(16) 2_565
Cu1 S1 2.3032(14) .
Cu1 S2 2.8078(14) .
S2 C10 1.703(4) .
S2 Cu1 2.2905(16) 2_565
S1 C1 1.720(4) .
S3 C11 1.710(5) .
N5 C11 1.370(6) .
N5 C13 1.392(6) .
N5 C12 1.453(6) .
N2 C1 1.334(6) .
N2 C4 1.381(6) .
N2 C5 1.476(6) .
N4 C10 1.345(6) .
N4 C8 1.376(6) .
N4 C9 1.478(6) .
N6 C11 1.348(6) .
N6 C14 1.391(6) .
N6 C15 1.464(6) .
N3 C10 1.367(6) .
N3 C7 1.388(6) .
N3 C6 1.450(6) .
N1 C1 1.339(6) .
N1 C3 1.376(6) .
N1 C2 1.472(7) .
C6 C5 1.520(7) .
C12 C12 1.552(8) 2_666
C13 C14 1.340(7) .
C4 C3 1.332(8) .
C8 C7 1.346(8) .
F1 B1 1.397(6) .
F2 B1 1.344(6) .
B1 F3 1.300(7) .
B1 F4 1.325(8) .
