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#$Date: 2016-03-21 11:04:52 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178679 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/90/4079035.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_4079035
loop_
_publ_author_name
'Ye, Qiong'
'Liu, Ming-Liang'
'Chen, Zi-Qi'
'Sun, Su-Wen'
'Xiong, Ren-Gen'
_publ_section_title
;
 Solvothermal Syntheses and Physical Properties of Noncentrosymmetric
 Olefin--Copper(I) Coordination Compounds
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              7862
_journal_paper_doi               10.1021/om300343j
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C30 H50 Br11 Cu8 N3 O'
_chemical_formula_weight         1856.06
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           146
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   12.1250(9)
_cell_length_b                   12.1250(9)
_cell_length_c                   29.3362(17)
_cell_measurement_temperature    293(2)
_cell_volume                     3735.1(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0764
_diffrn_reflns_av_sigmaI/netI    0.0621
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            12779
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.36
_exptl_absorpt_coefficient_mu    12.201
_exptl_crystal_density_diffrn    2.476
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2628
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.814
_refine_diff_density_min         -0.892
_refine_diff_density_rms         0.156
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         3813
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0506
_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)+(0.0708P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1243
_reflns_number_gt                3220
_reflns_number_total             3813
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300343j_si_001.cif
_cod_data_source_block           compound2
_cod_database_code               4079035
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
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
Br5 Br 0.75053(9) 0.60782(10) 0.74020(3) 0.0490(2) Uani 1 1 d .
Br4 Br 0.87303(9) 0.77970(8) 0.86019(3) 0.0455(2) Uani 1 1 d .
Br3 Br 1.0000 1.0000 0.74355(4) 0.0412(3) Uani 1 3 d S
Br2 Br 1.0000 1.0000 0.98318(5) 0.0464(4) Uani 1 3 d S
Br1 Br 0.90762(10) 0.47663(9) 0.84076(3) 0.0485(2) Uani 1 1 d .
Cu4 Cu 1.0000 1.0000 0.82294(9) 0.0844(9) Uani 1 3 d SU
Cu3 Cu 0.73289(14) 0.49596(16) 0.81626(5) 0.0672(4) Uani 1 1 d .
Cu2 Cu 1.0000 1.0000 0.905(9) 0.1443(19) Uani 0.50 3 d SPU
Cu2' Cu 1.0000 1.0000 0.905(9) 0.1443(19) Uani 0.50 3 d SPU
Cu1 Cu 0.93906(13) 0.74570(16) 0.78456(4) 0.0633(4) Uani 1 1 d .
N1 N 1.0026(6) 0.7029(6) 0.6707(2) 0.0306(13) Uani 1 1 d .
H1B H 0.9294 0.6936 0.6829 0.037 Uiso 1 1 calc R
C10 C 1.1097(8) 0.7764(8) 0.7042(3) 0.0368(17) Uani 1 1 d .
H10A H 1.1277 0.8631 0.7051 0.044 Uiso 1 1 d R
H10B H 1.1847 0.7770 0.6934 0.044 Uiso 1 1 d R
C9 C 0.7740(8) 0.7432(7) 0.6245(3) 0.0351(16) Uani 1 1 d .
H9A H 0.6983 0.7497 0.6247 0.053 Uiso 1 1 calc R
H9B H 0.7727 0.6930 0.6500 0.053 Uiso 1 1 calc R
H9C H 0.7777 0.7034 0.5967 0.053 Uiso 1 1 calc R
C8 C 0.8916(7) 0.8770(7) 0.6278(2) 0.0291(15) Uani 1 1 d .
C7 C 1.0144(7) 0.8924(6) 0.6282(2) 0.0235(14) Uani 1 1 d .
C6 C 1.0279(8) 0.7750(7) 0.6258(3) 0.0320(15) Uani 1 1 d .
H6A H 0.9690 0.7185 0.6034 0.038 Uiso 1 1 d R
H6B H 1.1123 0.7993 0.6156 0.038 Uiso 1 1 d R
C5 C 0.8957(14) 0.4594(11) 0.5903(4) 0.069(3) Uani 1 1 d .
H5A H 0.9808 0.4827 0.5813 0.083 Uiso 1 1 d R
H5B H 0.8258 0.4115 0.5699 0.083 Uiso 1 1 d R
C4 C 0.8763(10) 0.4932(10) 0.6301(4) 0.052(2) Uani 1 1 d .
H4A H 0.7912 0.4699 0.6390 0.063 Uiso 1 1 d R
C3 C 1.1311(9) 0.7971(10) 0.7895(3) 0.051(2) Uani 1 1 d .
H3A H 1.1536 0.7609 0.8145 0.061 Uiso 1 1 d R
H3B H 1.1922 0.8850 0.7840 0.061 Uiso 1 1 d R
C2 C 0.9844(9) 0.5686(8) 0.6626(3) 0.0430(19) Uani 1 1 d .
H2A H 0.9678 0.5247 0.6913 0.052 Uiso 1 1 d R
H2B H 1.0611 0.5762 0.6502 0.052 Uiso 1 1 d R
C1 C 1.0816(9) 0.7231(8) 0.7522(3) 0.0418(19) Uani 1 1 d .
H1A H 1.0708 0.6394 0.7550 0.050 Uiso 1 1 d R
O1W O 1.3333 0.6667 0.805(3) 0.42(5) Uani 1 3 d S
H1WA H 1.4105 0.7263 0.8053 0.623 Uiso 0.33 1 d PR
H1WB H 1.3155 0.6247 0.8294 0.623 Uiso 0.33 1 d PR
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'
Br Br -0.2901 2.4595 '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'
N N 0.0061 0.0033 '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'
O O 0.0106 0.0060 '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
Cu1 Br5 Cu3 72.45(6) . .
Cu1 Br4 Cu4 73.41(7) . .
Cu1 Br4 Cu2 123(4) . .
Cu4 Br4 Cu2 55(5) . .
Cu1 Br4 Cu2' 123(4) . .
Cu4 Br4 Cu2' 55(5) . .
Cu2 Br4 Cu2' 0(9) . .
Cu2' Br2 Cu2 0.00(5) . .
Cu3 Br1 Cu3 78.10(9) . 3_665
Br3 Cu4 Cu2 180.00(9) . .
Br3 Cu4 Cu2' 180.00(9) . .
Cu2 Cu4 Cu2' 0.00(5) . .
Br3 Cu4 Br4 115.20(6) . 2_765
Cu2 Cu4 Br4 64.80(7) . 2_765
Cu2' Cu4 Br4 64.80(7) . 2_765
Br3 Cu4 Br4 115.20(6) . .
Cu2 Cu4 Br4 64.80(7) . .
Cu2' Cu4 Br4 64.80(7) . .
Br4 Cu4 Br4 103.18(7) 2_765 .
Br3 Cu4 Br4 115.20(6) . 3_675
Cu2 Cu4 Br4 64.80(6) . 3_675
Cu2' Cu4 Br4 64.80(6) . 3_675
Br4 Cu4 Br4 103.18(7) 2_765 3_675
Br4 Cu4 Br4 103.18(7) . 3_675
Br3 Cu4 Cu1 68.01(5) . .
Cu2 Cu4 Cu1 111.99(6) . .
Cu2' Cu4 Cu1 111.99(6) . .
Br4 Cu4 Cu1 106.23(3) 2_765 .
Br4 Cu4 Cu1 51.71(3) . .
Br4 Cu4 Cu1 144.93(4) 3_675 .
Br3 Cu4 Cu1 68.01(5) . 2_765
Cu2 Cu4 Cu1 111.99(7) . 2_765
Cu2' Cu4 Cu1 111.99(7) . 2_765
Br4 Cu4 Cu1 51.71(3) 2_765 2_765
Br4 Cu4 Cu1 144.93(3) . 2_765
Br4 Cu4 Cu1 106.23(4) 3_675 2_765
Cu1 Cu4 Cu1 106.84(6) . 2_765
Br3 Cu4 Cu1 68.01(5) . 3_675
Cu2 Cu4 Cu1 111.99(6) . 3_675
Cu2' Cu4 Cu1 111.99(6) . 3_675
Br4 Cu4 Cu1 144.93(4) 2_765 3_675
Br4 Cu4 Cu1 106.23(4) . 3_675
Br4 Cu4 Cu1 51.71(3) 3_675 3_675
Cu1 Cu4 Cu1 106.84(6) . 3_675
Cu1 Cu4 Cu1 106.84(6) 2_765 3_675
Br1 Cu3 Br1 138.04(9) . 2_655
Br1 Cu3 Br5 118.46(7) . .
Br1 Cu3 Br5 103.43(6) 2_655 .
Br1 Cu3 Cu1 81.71(6) . .
Br1 Cu3 Cu1 130.94(8) 2_655 .
Br5 Cu3 Cu1 51.63(4) . .
Br1 Cu3 Cu3 107.78(6) . 2_655
Br1 Cu3 Cu3 50.84(6) 2_655 2_655
Br5 Cu3 Cu3 110.21(5) . 2_655
Cu1 Cu3 Cu3 161.35(4) . 2_655
Br1 Cu3 Cu3 51.05(6) . 3_665
Br1 Cu3 Cu3 107.58(6) 2_655 3_665
Br5 Cu3 Cu3 118.48(5) . 3_665
Cu1 Cu3 Cu3 121.39(8) . 3_665
Cu3 Cu3 Cu3 60.000(1) 2_655 3_665
Br2 Cu2 Cu4 180.000(1) . .
Br2 Cu2 Br4 120(5) . .
Cu4 Cu2 Br4 60(5) . .
Br2 Cu2 Br4 120(5) . 2_765
Cu4 Cu2 Br4 60(5) . 2_765
Br4 Cu2 Br4 98(6) . 2_765
Br2 Cu2 Br4 120(5) . 3_675
Cu4 Cu2 Br4 60(5) . 3_675
Br4 Cu2 Br4 98(6) . 3_675
Br4 Cu2 Br4 98(6) 2_765 3_675
Br2 Cu2' Cu4 180.000(1) . .
Br2 Cu2' Br4 120(5) . .
Cu4 Cu2' Br4 60(5) . .
Br2 Cu2' Br4 120(5) . 2_765
Cu4 Cu2' Br4 60(5) . 2_765
Br4 Cu2' Br4 98(6) . 2_765
Br2 Cu2' Br4 120(5) . 3_675
Cu4 Cu2' Br4 60(5) . 3_675
Br4 Cu2' Br4 98(6) . 3_675
Br4 Cu2' Br4 98(6) 2_765 3_675
C3 Cu1 C1 37.5(4) . .
C3 Cu1 Br5 140.1(3) . .
C1 Cu1 Br5 102.8(3) . .
C3 Cu1 Br4 107.1(3) . .
C1 Cu1 Br4 141.6(3) . .
Br5 Cu1 Br4 108.98(6) . .
C3 Cu1 Cu3 121.9(3) . .
C1 Cu1 Cu3 109.7(3) . .
Br5 Cu1 Cu3 55.91(5) . .
Br4 Cu1 Cu3 73.05(5) . .
C3 Cu1 Cu4 90.1(3) . .
C1 Cu1 Cu4 120.3(3) . .
Br5 Cu1 Cu4 124.81(7) . .
Br4 Cu1 Cu4 54.88(6) . .
Cu3 Cu1 Cu4 125.57(6) . .
C10 N1 C6 110.8(6) . .
C10 N1 C2 110.4(6) . .
C6 N1 C2 110.6(6) . .
C10 N1 H1B 108.3 . .
C6 N1 H1B 108.3 . .
C2 N1 H1B 108.3 . .
N1 C10 C1 114.1(7) . .
N1 C10 H10A 108.8 . .
C1 C10 H10A 108.7 . .
N1 C10 H10B 108.7 . .
C1 C10 H10B 108.6 . .
H10A C10 H10B 107.8 . .
C8 C9 H9A 109.5 . .
C8 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C8 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C7 C8 C7 119.2(7) 3_675 .
C7 C8 C9 120.5(7) 3_675 .
C7 C8 C9 120.2(6) . .
C8 C7 C8 120.8(7) 2_765 .
C8 C7 C6 120.4(7) 2_765 .
C8 C7 C6 118.7(6) . .
C7 C6 N1 114.5(6) . .
C7 C6 H6A 108.1 . .
N1 C6 H6A 108.6 . .
C7 C6 H6B 108.9 . .
N1 C6 H6B 108.8 . .
H6A C6 H6B 107.7 . .
C4 C5 H5A 119.5 . .
C4 C5 H5B 120.5 . .
H5A C5 H5B 120.0 . .
C5 C4 C2 121.5(11) . .
C5 C4 H4A 119.3 . .
C2 C4 H4A 119.2 . .
C1 C3 Cu1 71.8(6) . .
C1 C3 H3A 116.5 . .
Cu1 C3 H3A 116.5 . .
C1 C3 H3B 116.1 . .
Cu1 C3 H3B 116.4 . .
H3A C3 H3B 113.5 . .
C4 C2 N1 111.0(7) . .
C4 C2 H2A 109.9 . .
N1 C2 H2A 109.2 . .
C4 C2 H2B 108.9 . .
N1 C2 H2B 109.7 . .
H2A C2 H2B 108.1 . .
C3 C1 C10 122.6(8) . .
C3 C1 Cu1 70.7(6) . .
C10 C1 Cu1 112.7(6) . .
C3 C1 H1A 114.5 . .
C10 C1 H1A 114.4 . .
Cu1 C1 H1A 114.4 . .
H1WA O1W H1WB 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br5 Cu1 2.4274(17) .
Br5 Cu3 2.5640(19) .
Br4 Cu1 2.4626(15) .
Br4 Cu4 2.5666(14) .
Br4 Cu2 2.67(13) .
Br4 Cu2' 2.67(13) .
Br3 Cu4 2.329(3) .
Br2 Cu2' 2.3(3) .
Br2 Cu2 2.3(3) .
Br1 Cu3 2.3573(18) .
Br1 Cu3 2.3643(17) 3_665
Cu4 Cu2 2.4(3) .
Cu4 Cu2' 2.4(3) .
Cu4 Br4 2.5666(14) 2_765
Cu4 Br4 2.5666(14) 3_675
Cu4 Cu1 3.0071(19) .
Cu4 Cu1 3.007(2) 2_765
Cu4 Cu1 3.0071(19) 3_675
Cu3 Br1 2.3643(17) 2_655
Cu3 Cu1 2.952(2) .
Cu3 Cu3 2.975(3) 2_655
Cu3 Cu3 2.975(3) 3_665
Cu2 Br4 2.67(13) 2_765
Cu2 Br4 2.67(13) 3_675
Cu2' Br4 2.67(13) 2_765
Cu2' Br4 2.67(13) 3_675
Cu1 C3 2.093(10) .
Cu1 C1 2.106(10) .
N1 C10 1.513(11) .
N1 C6 1.525(10) .
N1 C2 1.548(10) .
N1 H1B 0.9100 .
C10 C1 1.517(12) .
C10 H10A 0.9601 .
C10 H10B 0.9599 .
C9 C8 1.536(11) .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C8 C7 1.406(10) 3_675
C8 C7 1.406(10) .
C7 C8 1.406(10) 2_765
C7 C6 1.513(10) .
C6 H6A 0.9600 .
C6 H6B 0.9600 .
C5 C4 1.297(17) .
C5 H5A 0.9599 .
C5 H5B 0.9600 .
C4 C2 1.506(14) .
C4 H4A 0.9600 .
C3 C1 1.350(14) .
C3 H3A 0.9598 .
C3 H3B 0.9600 .
C2 H2A 0.9604 .
C2 H2B 0.9600 .
C1 H1A 0.9600 .
O1W H1WA 0.8500 .
O1W H1WB 0.8498 .
