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#$Date: 2016-03-21 19:04:36 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178834 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/88/4108802.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_4108802
loop_
_publ_author_name
'Marie Sircoglou'
'Sébastien Bontemps'
'Ghenwa Bouhadir'
'Nathalie Saffon'
'Karinne Miqueu'
'Weixing Gu'
'Maxime Mercy'
'Chun-Hsing Chen'
'Bruce M. Foxman'
'Laurent Maron'
'Oleg V. Ozerov'
'Didier Bourissou'
_publ_section_title
;
 Group 10 and 11 Metal Boratranes (Ni, Pd, Pt, CuCl, AgCl, AuCl, and Au+)
 Derived from a Triphosphine-Borane
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16729
_journal_page_last               16738
_journal_paper_doi               10.1021/ja8070072
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C39 H60 B Cl7 Cu P3'
_chemical_formula_weight         944.28
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_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            6
_cell_length_a                   17.7510(4)
_cell_length_b                   17.7510(4)
_cell_length_c                   25.1600(12)
_cell_measurement_reflns_used    9988
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.439
_cell_measurement_theta_min      2.294
_cell_volume                     6865.7(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0142
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            23149
_diffrn_reflns_theta_full        29.57
_diffrn_reflns_theta_max         29.57
_diffrn_reflns_theta_min         5.20
_exptl_absorpt_coefficient_mu    1.018
_exptl_absorpt_correction_T_max  0.7499
_exptl_absorpt_correction_T_min  0.5360
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_description       block
_exptl_crystal_F_000             2952
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         4264
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0252
_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)+(0.0339P)²+7.1234P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0691
_reflns_number_gt                3815
_reflns_number_total             4264
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8070072_si_005.cif
_cod_data_source_block           marie3m
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4108802
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'
'-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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.6667 0.3333 0.109391(9) 0.01600(6) Uani 1 3 d S . .
Cl1 Cl 0.6667 0.3333 0.015321(18) 0.02397(10) Uani 1 3 d S . .
P1 P 0.581766(18) 0.399220(18) 0.125323(11) 0.01726(7) Uani 1 1 d . . .
B1 B 0.6667 0.3333 0.20907(8) 0.0171(4) Uani 1 3 d SU . .
C1 C 0.57566(7) 0.32700(7) 0.22251(4) 0.0182(2) Uani 1 1 d U . .
C2 C 0.53357(7) 0.35960(7) 0.19057(4) 0.0185(2) Uani 1 1 d U . .
C3 C 0.45754(8) 0.35709(8) 0.20828(5) 0.0251(2) Uani 1 1 d U . .
H3 H 0.4297 0.3795 0.1863 0.030 Uiso 1 1 calc R . .
C4 C 0.42239(8) 0.32210(10) 0.25774(5) 0.0310(3) Uani 1 1 d U . .
H4 H 0.3713 0.3215 0.2698 0.037 Uiso 1 1 calc R . .
C5 C 0.46210(8) 0.28827(9) 0.28931(5) 0.0301(3) Uani 1 1 d U . .
H5 H 0.4380 0.2635 0.3229 0.036 Uiso 1 1 calc R . .
C6 C 0.53760(8) 0.29070(8) 0.27158(4) 0.0242(2) Uani 1 1 d U . .
H6 H 0.5642 0.2670 0.2935 0.029 Uiso 1 1 calc R . .
C7 C 0.48719(8) 0.36281(8) 0.07969(5) 0.0230(2) Uani 1 1 d U . .
H7 H 0.4468 0.3804 0.0958 0.028 Uiso 1 1 calc R . .
C8 C 0.43686(9) 0.26425(9) 0.07279(6) 0.0320(3) Uani 1 1 d U . .
H8A H 0.3874 0.2479 0.0489 0.048 Uiso 1 1 calc R . .
H8B H 0.4155 0.2365 0.1074 0.048 Uiso 1 1 calc R . .
H8C H 0.4753 0.2450 0.0576 0.048 Uiso 1 1 calc R . .
C9 C 0.51547(10) 0.40711(10) 0.02528(5) 0.0324(3) Uani 1 1 d U . .
H9A H 0.5522 0.3881 0.0075 0.049 Uiso 1 1 calc R . .
H9B H 0.5483 0.4704 0.0300 0.049 Uiso 1 1 calc R . .
H9C H 0.4639 0.3912 0.0035 0.049 Uiso 1 1 calc R . .
C10 C 0.62389(8) 0.51916(7) 0.12905(5) 0.0242(2) Uani 1 1 d U . .
H10 H 0.6604 0.5459 0.0967 0.029 Uiso 1 1 calc R . .
C11 C 0.68303(9) 0.55901(8) 0.17732(6) 0.0309(3) Uani 1 1 d U . .
H11A H 0.7092 0.6224 0.1764 0.046 Uiso 1 1 calc R . .
H11B H 0.7291 0.5439 0.1766 0.046 Uiso 1 1 calc R . .
H11C H 0.6488 0.5363 0.2099 0.046 Uiso 1 1 calc R . .
C12 C 0.55391(9) 0.54580(9) 0.12985(6) 0.0331(3) Uani 1 1 d U . .
H12A H 0.5179 0.5221 0.1617 0.050 Uiso 1 1 calc R . .
H12B H 0.5173 0.5229 0.0981 0.050 Uiso 1 1 calc R . .
H12C H 0.5819 0.6094 0.1302 0.050 Uiso 1 1 calc R . .
C13 C 0.19847(11) 0.69447(11) 0.07710(7) 0.0462(4) Uani 1 1 d DU . .
H13A H 0.2228 0.6810 0.0454 0.055 Uiso 1 1 calc R A 1
H13B H 0.1806 0.6462 0.1028 0.055 Uiso 1 1 calc R A 1
Cl2 Cl 0.2802(2) 0.7919(3) 0.1063(3) 0.0529(8) Uani 0.54(2) 1 d PDU B 1
Cl3 Cl 0.1082(2) 0.7006(4) 0.0584(3) 0.0607(8) Uani 0.54(2) 1 d PDU B 1
Cl2' Cl 0.2808(4) 0.7830(5) 0.1095(4) 0.0739(16) Uani 0.46(2) 1 d PDU B 2
Cl3' Cl 0.1164(4) 0.7149(5) 0.0520(2) 0.0618(9) Uani 0.46(2) 1 d PDU B 2
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'
P P 0.1023 0.0942 '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'
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
P1 Cu1 P1 117.172(5) 3_665 2_655
P1 Cu1 P1 117.172(5) 3_665 .
P1 Cu1 P1 117.172(5) 2_655 .
P1 Cu1 Cl1 99.786(8) 3_665 .
P1 Cu1 Cl1 99.786(8) 2_655 .
P1 Cu1 Cl1 99.786(8) . .
P1 Cu1 B1 80.214(8) 3_665 .
P1 Cu1 B1 80.214(8) 2_655 .
P1 Cu1 B1 80.214(8) . .
Cl1 Cu1 B1 180.0 . .
C2 P1 C7 104.69(5) . .
C2 P1 C10 103.72(5) . .
C7 P1 C10 101.75(5) . .
C2 P1 Cu1 104.77(4) . .
C7 P1 Cu1 114.31(4) . .
C10 P1 Cu1 125.54(4) . .
C1 B1 C1 115.65(5) 2_655 3_665
C1 B1 C1 115.65(5) 2_655 .
C1 B1 C1 115.65(5) 3_665 .
C1 B1 Cu1 102.21(8) 2_655 .
C1 B1 Cu1 102.21(8) 3_665 .
C1 B1 Cu1 102.21(8) . .
C6 C1 C2 117.43(10) . .
C6 C1 B1 117.19(11) . .
C2 C1 B1 125.26(10) . .
C3 C2 C1 120.50(10) . .
C3 C2 P1 123.91(9) . .
C1 C2 P1 115.52(8) . .
C4 C3 C2 120.57(11) . .
C5 C4 C3 119.70(11) . .
C4 C5 C6 119.62(11) . .
C5 C6 C1 122.15(11) . .
C8 C7 C9 109.91(11) . .
C8 C7 P1 112.18(8) . .
C9 C7 P1 111.43(9) . .
C11 C10 C12 108.76(11) . .
C11 C10 P1 110.94(8) . .
C12 C10 P1 115.24(9) . .
Cl2' C13 Cl3 117.5(3) . .
Cl2' C13 Cl2 5.8(6) . .
Cl3 C13 Cl2 112.7(2) . .
Cl2' C13 Cl3' 112.8(3) . .
Cl3 C13 Cl3' 8.8(3) . .
Cl2 C13 Cl3' 107.6(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 P1 2.3585(3) 3_665
Cu1 P1 2.3585(3) 2_655
Cu1 P1 2.3585(3) .
Cu1 Cl1 2.3668(5) .
Cu1 B1 2.508(2) .
P1 C2 1.8220(11) .
P1 C7 1.8626(12) .
P1 C10 1.8731(12) .
B1 C1 1.5985(11) 2_655
B1 C1 1.5985(12) 3_665
B1 C1 1.5985(11) .
C1 C6 1.4002(15) .
C1 C2 1.4041(15) .
C2 C3 1.4007(15) .
C3 C4 1.3914(17) .
C4 C5 1.3827(19) .
C5 C6 1.3925(17) .
C7 C8 1.5251(18) .
C7 C9 1.5328(17) .
C10 C11 1.5281(19) .
C10 C12 1.5345(17) .
C13 Cl2' 1.724(6) .
C13 Cl3 1.724(5) .
C13 Cl2 1.768(4) .
C13 Cl3' 1.784(5) .
