#------------------------------------------------------------------------------
#$Date: 2016-03-21 11:04:52 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178679 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/90/4079034.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_4079034
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 H48 Cl7 Cu4 N3'
_chemical_formula_weight         953.02
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           161
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :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            6
_cell_length_a                   14.233(2)
_cell_length_b                   14.233(2)
_cell_length_c                   40.08(4)
_cell_measurement_temperature    293(2)
_cell_volume                     7032(7)
_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  0.0510
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            23216
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         2.86
_exptl_absorpt_coefficient_mu    2.210
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2904
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.918
_refine_diff_density_min         -0.869
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         3735
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0707
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1144P)²+18.5193P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1965
_refine_ls_wR_factor_ref         0.2032
_reflns_number_gt                3333
_reflns_number_total             3735
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300343j_si_001.cif
_cod_data_source_block           compound_1
_cod_original_sg_symbol_H-M      R3c
_cod_database_code               4079034
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'x, x-y, z+1/2'
'-x+y, y, z+1/2'
'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'
'-y+2/3, -x+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'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'
'-y+1/3, -x+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
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 0.6667 0.3333 -0.04017(5) 0.0646(4) Uani 1 3 d S
Cu2 Cu 0.52428(8) 0.40382(8) -0.00663(2) 0.0624(3) Uani 1 1 d .
Cl3 Cl 0.58487(18) 0.55806(19) 0.02324(5) 0.0702(5) Uiso 1 1 d .
Cl2 Cl 0.60098(16) 0.44572(16) -0.05863(5) 0.0622(4) Uani 1 1 d .
Cl1 Cl 0.6667 0.3333 0.01902(7) 0.0501(6) Uani 1 3 d S
N1 N 0.4344(4) 0.3678(4) 0.07463(15) 0.0485(12) Uani 1 1 d .
H1B H 0.4938 0.4254 0.0655 0.058 Uiso 1 1 calc R
C10 C 0.367(2) 0.5310(18) 0.1249(8) 0.25(2) Uani 1 1 d .
H10A H 0.3116 0.4771 0.1376 0.302 Uiso 1 1 calc R
H10B H 0.4033 0.6023 0.1325 0.302 Uiso 1 1 calc R
C9 C 0.3934(9) 0.5078(9) 0.0979(3) 0.088(3) Uani 1 1 d .
H9A H 0.4496 0.5660 0.0867 0.106 Uiso 1 1 calc R
C8 C 0.3931(6) 0.2505(6) -0.0100(2) 0.0602(17) Uani 1 1 d .
H8A H 0.3459 0.2361 -0.0291 0.072 Uiso 1 1 calc R
H8B H 0.4060 0.1913 -0.0048 0.072 Uiso 1 1 calc R
C7 C 0.3971(5) 0.2749(5) 0.05196(17) 0.0487(13) Uani 1 1 d .
H7A H 0.3305 0.2149 0.0607 0.058 Uiso 1 1 calc R
H7B H 0.4511 0.2524 0.0513 0.058 Uiso 1 1 calc R
C6 C 0.3481(7) 0.4000(8) 0.0804(3) 0.071(2) Uani 1 1 d .
H6A H 0.3179 0.4038 0.0591 0.085 Uiso 1 1 calc R
H6B H 0.2899 0.3446 0.0937 0.085 Uiso 1 1 calc R
C5 C 0.4580(6) 0.1316(6) 0.1094(2) 0.0578(16) Uani 1 1 d .
H5A H 0.3996 0.1470 0.1094 0.087 Uiso 1 1 calc R
H5B H 0.4561 0.0946 0.1297 0.087 Uiso 1 1 calc R
H5C H 0.4504 0.0864 0.0906 0.087 Uiso 1 1 calc R
C4 C 0.5692(5) 0.3360(5) 0.10655(14) 0.0418(11) Uani 1 1 d .
C3 C 0.4667(5) 0.3418(5) 0.10817(15) 0.0482(13) Uani 1 1 d .
H3A H 0.4764 0.3971 0.1242 0.058 Uiso 1 1 calc R
H3B H 0.4082 0.2729 0.1161 0.058 Uiso 1 1 calc R
C2 C 0.5646(5) 0.2362(5) 0.10705(15) 0.0443(12) Uani 1 1 d .
C1 C 0.3766(5) 0.2995(5) 0.01623(17) 0.0507(14) Uani 1 1 d .
H1A H 0.3193 0.3180 0.0136 0.061 Uiso 1 1 calc R
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'
Cl Cl 0.1484 0.1585 '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'
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
Cl2 Cu1 Cl2 110.49(7) 3_665 2_655
Cl2 Cu1 Cl2 110.49(7) 3_665 .
Cl2 Cu1 Cl2 110.49(7) 2_655 .
Cl2 Cu1 Cl1 108.44(7) 3_665 .
Cl2 Cu1 Cl1 108.44(7) 2_655 .
Cl2 Cu1 Cl1 108.44(7) . .
Cl2 Cu1 Cu2 107.12(6) 3_665 2_655
Cl2 Cu1 Cu2 48.99(6) 2_655 2_655
Cl2 Cu1 Cu2 141.99(5) . 2_655
Cl1 Cu1 Cu2 63.31(5) . 2_655
Cl2 Cu1 Cu2 48.99(6) 3_665 3_665
Cl2 Cu1 Cu2 141.99(5) 2_655 3_665
Cl2 Cu1 Cu2 107.12(6) . 3_665
Cl1 Cu1 Cu2 63.31(5) . 3_665
Cu2 Cu1 Cu2 101.38(6) 2_655 3_665
Cl2 Cu1 Cu2 141.99(5) 3_665 .
Cl2 Cu1 Cu2 107.12(6) 2_655 .
Cl2 Cu1 Cu2 48.99(6) . .
Cl1 Cu1 Cu2 63.31(5) . .
Cu2 Cu1 Cu2 101.38(6) 2_655 .
Cu2 Cu1 Cu2 101.38(6) 3_665 .
C8 Cu2 C1 38.0(3) . .
C8 Cu2 Cl3 140.5(2) . .
C1 Cu2 Cl3 102.6(2) . .
C8 Cu2 Cl2 106.3(2) . .
C1 Cu2 Cl2 140.0(2) . .
Cl3 Cu2 Cl2 109.19(9) . .
C8 Cu2 Cu1 91.3(2) . .
C1 Cu2 Cu1 124.7(2) . .
Cl3 Cu2 Cu1 124.78(7) . .
Cl2 Cu2 Cu1 50.48(6) . .
Cu2 Cl2 Cu1 80.53(8) . .
C7 N1 C3 110.1(5) . .
C7 N1 C6 112.4(6) . .
C3 N1 C6 108.9(6) . .
C7 N1 H1B 108.4 . .
C3 N1 H1B 108.4 . .
C6 N1 H1B 108.4 . .
C9 C10 H10A 120.0 . .
C9 C10 H10B 120.0 . .
H10A C10 H10B 120.0 . .
C10 C9 C6 130.1(15) . .
C10 C9 H9A 115.0 . .
C6 C9 H9A 115.0 . .
C1 C8 Cu2 72.5(4) . .
C1 C8 H8A 116.3 . .
Cu2 C8 H8A 116.3 . .
C1 C8 H8B 116.3 . .
Cu2 C8 H8B 116.3 . .
H8A C8 H8B 113.3 . .
N1 C7 C1 113.3(5) . .
N1 C7 H7A 108.9 . .
C1 C7 H7A 108.9 . .
N1 C7 H7B 108.9 . .
C1 C7 H7B 108.9 . .
H7A C7 H7B 107.7 . .
C9 C6 N1 112.2(7) . .
C9 C6 H6A 109.2 . .
N1 C6 H6A 109.2 . .
C9 C6 H6B 109.2 . .
N1 C6 H6B 109.2 . .
H6A C6 H6B 107.9 . .
C2 C5 H5A 109.5 . .
C2 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C2 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
C2 C4 C2 120.8(6) . 3_665
C2 C4 C3 120.4(5) . .
C2 C4 C3 118.7(5) 3_665 .
C4 C3 N1 113.2(5) . .
C4 C3 H3A 108.9 . .
N1 C3 H3A 108.9 . .
C4 C3 H3B 108.9 . .
N1 C3 H3B 108.9 . .
H3A C3 H3B 107.7 . .
C4 C2 C4 119.2(6) . 2_655
C4 C2 C5 121.3(6) . .
C4 C2 C5 119.4(5) 2_655 .
C8 C1 C7 120.5(6) . .
C8 C1 Cu2 69.5(4) . .
C7 C1 Cu2 109.5(4) . .
C8 C1 H1A 116.1 . .
C7 C1 H1A 116.1 . .
Cu2 C1 H1A 116.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 Cl2 2.3401(18) 3_665
Cu1 Cl2 2.3401(18) 2_655
Cu1 Cl2 2.3401(18) .
Cu1 Cl1 2.372(4) .
Cu1 Cu2 2.9922(15) 2_655
Cu1 Cu2 2.9922(15) 3_665
Cu1 Cu2 2.9922(15) .
Cu2 C8 2.048(7) .
Cu2 C1 2.084(6) .
Cu2 Cl3 2.259(2) .
Cu2 Cl2 2.289(3) .
N1 C7 1.468(9) .
N1 C3 1.525(9) .
N1 C6 1.527(8) .
N1 H1B 0.9100 .
C10 C9 1.24(2) .
C10 H10A 0.9300 .
C10 H10B 0.9300 .
C9 C6 1.507(14) .
C9 H9A 0.9300 .
C8 C1 1.345(11) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C7 C1 1.537(9) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C5 C2 1.506(9) .
C5 H5A 0.9600 .
C5 H5B 0.9600 .
C5 H5C 0.9600 .
C4 C2 1.390(9) .
C4 C2 1.436(8) 3_665
C4 C3 1.502(9) .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C2 C4 1.436(8) 2_655
C1 H1A 0.9800 .
