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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/4/10/88/4108801.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_4108801
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 Ag B Cl7 P3'
_chemical_formula_weight         988.61
_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                   17.8985(4)
_cell_length_b                   17.8985(4)
_cell_length_c                   25.1626(11)
_cell_measurement_reflns_used    9889
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      31.59
_cell_measurement_theta_min      2.28
_cell_volume                     6981.0(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  0.0228
_diffrn_reflns_av_sigmaI/netI    0.0169
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            21221
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         5.16
_exptl_absorpt_coefficient_mu    0.965
_exptl_absorpt_correction_T_max  0.7606
_exptl_absorpt_correction_T_min  0.5515
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_description       block
_exptl_crystal_F_000             3060
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         3825
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0242
_refine_ls_R_factor_gt           0.0199
_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)+(0.0259P)²+6.7744P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0509
_refine_ls_wR_factor_ref         0.0531
_reflns_number_gt                3433
_reflns_number_total             3825
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8070072_si_004.cif
_cod_data_source_block           marie6m
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4108801
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
Ag1 Ag 0.6667 0.3333 0.107889(6) 0.01696(5) Uani 1 3 d S . .
Cl1 Cl 0.6667 0.3333 0.00537(2) 0.02760(12) Uani 1 3 d S . .
P1 P 0.57843(2) 0.40320(2) 0.126197(12) 0.01876(7) Uani 1 1 d . . .
B1 B 0.6667 0.3333 0.20885(9) 0.0182(4) Uani 1 3 d S . .
C1 C 0.57592(8) 0.32692(7) 0.22211(5) 0.0190(2) Uani 1 1 d . . .
C2 C 0.53428(8) 0.36159(8) 0.19188(5) 0.0198(2) Uani 1 1 d . . .
C3 C 0.45944(9) 0.35870(9) 0.21105(6) 0.0274(3) Uani 1 1 d . . .
H3 H 0.4320 0.3825 0.1903 0.033 Uiso 1 1 calc R . .
C4 C 0.42485(9) 0.32157(11) 0.25990(6) 0.0329(3) Uani 1 1 d . . .
H4 H 0.3745 0.3207 0.2728 0.039 Uiso 1 1 calc R . .
C5 C 0.46407(9) 0.28589(10) 0.28964(6) 0.0313(3) Uani 1 1 d . . .
H5 H 0.4403 0.2596 0.3229 0.038 Uiso 1 1 calc R . .
C6 C 0.53814(8) 0.28850(9) 0.27092(5) 0.0251(3) Uani 1 1 d . . .
H6 H 0.5642 0.2635 0.2918 0.030 Uiso 1 1 calc R . .
C7 C 0.48351(8) 0.36449(9) 0.08175(5) 0.0244(3) Uani 1 1 d . . .
H7 H 0.4431 0.3818 0.0974 0.029 Uiso 1 1 calc R . .
C8 C 0.43563(10) 0.26626(10) 0.07628(6) 0.0340(3) Uani 1 1 d . . .
H8A H 0.3854 0.2478 0.0531 0.051 Uiso 1 1 calc R . .
H8B H 0.4164 0.2398 0.1114 0.051 Uiso 1 1 calc R . .
H8C H 0.4743 0.2482 0.0608 0.051 Uiso 1 1 calc R . .
C9 C 0.51186(11) 0.40656(11) 0.02693(6) 0.0356(3) Uani 1 1 d . . .
H9A H 0.5502 0.3888 0.0105 0.053 Uiso 1 1 calc R . .
H9B H 0.5425 0.4695 0.0308 0.053 Uiso 1 1 calc R . .
H9C H 0.4610 0.3883 0.0044 0.053 Uiso 1 1 calc R . .
C10 C 0.62035(9) 0.52172(8) 0.13009(6) 0.0266(3) Uani 1 1 d . . .
H10 H 0.6562 0.5482 0.0976 0.032 Uiso 1 1 calc R . .
C11 C 0.67999(10) 0.56022(9) 0.17792(7) 0.0338(3) Uani 1 1 d . . .
H11A H 0.7082 0.6233 0.1765 0.051 Uiso 1 1 calc R . .
H11B H 0.7239 0.5427 0.1772 0.051 Uiso 1 1 calc R . .
H11C H 0.6462 0.5394 0.2107 0.051 Uiso 1 1 calc R . .
C12 C 0.55149(10) 0.54881(10) 0.13134(7) 0.0376(3) Uani 1 1 d . . .
H12A H 0.5165 0.5261 0.1636 0.056 Uiso 1 1 calc R . .
H12B H 0.5143 0.5257 0.1000 0.056 Uiso 1 1 calc R . .
H12C H 0.5796 0.6119 0.1312 0.056 Uiso 1 1 calc R . .
C13 C 0.19575(12) 0.69373(12) 0.07900(8) 0.0486(4) Uani 1 1 d DU . .
H13A H 0.2190 0.6734 0.0502 0.058 Uiso 1 1 calc R A 1
H13B H 0.1747 0.6499 0.1076 0.058 Uiso 1 1 calc R A 1
Cl2 Cl 0.2806(3) 0.7926(3) 0.1046(2) 0.0527(11) Uani 0.52(3) 1 d PDU B 1
Cl3 Cl 0.1104(3) 0.7016(4) 0.0546(3) 0.0646(10) Uani 0.52(3) 1 d PDU B 1
Cl2' Cl 0.2794(4) 0.7850(5) 0.1063(3) 0.088(2) Uani 0.48(3) 1 d PDU B 2
Cl3' Cl 0.1181(4) 0.7153(5) 0.0491(2) 0.0686(10) Uani 0.48(3) 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'
Ag Ag -0.8971 1.1015 '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 Ag1 P1 116.681(5) 2_655 3_665
P1 Ag1 P1 116.681(5) 2_655 .
P1 Ag1 P1 116.681(5) 3_665 .
P1 Ag1 B1 79.377(8) 2_655 .
P1 Ag1 B1 79.377(8) 3_665 .
P1 Ag1 B1 79.377(8) . .
P1 Ag1 Cl1 100.623(8) 2_655 .
P1 Ag1 Cl1 100.623(8) 3_665 .
P1 Ag1 Cl1 100.623(8) . .
B1 Ag1 Cl1 180.0 . .
C2 P1 C7 105.38(6) . .
C2 P1 C10 105.23(6) . .
C7 P1 C10 103.23(6) . .
C2 P1 Ag1 102.47(4) . .
C7 P1 Ag1 113.07(4) . .
C10 P1 Ag1 125.67(4) . .
C1 B1 C1 115.79(6) 2_655 3_665
C1 B1 C1 115.79(6) 2_655 .
C1 B1 C1 115.79(6) 3_665 .
C1 B1 Ag1 102.00(9) 2_655 .
C1 B1 Ag1 102.00(9) 3_665 .
C1 B1 Ag1 102.00(9) . .
C6 C1 C2 117.18(11) . .
C6 C1 B1 116.05(12) . .
C2 C1 B1 126.58(12) . .
C3 C2 C1 120.34(11) . .
C3 C2 P1 122.60(10) . .
C1 C2 P1 116.95(9) . .
C4 C3 C2 120.83(13) . .
C5 C4 C3 119.56(13) . .
C4 C5 C6 119.93(13) . .
C5 C6 C1 122.14(13) . .
C8 C7 C9 109.98(12) . .
C8 C7 P1 111.46(9) . .
C9 C7 P1 110.07(10) . .
C11 C10 C12 109.41(12) . .
C11 C10 P1 110.35(9) . .
C12 C10 P1 115.51(10) . .
Cl2' C13 Cl3 117.0(3) . .
Cl2' C13 Cl2 3.8(4) . .
Cl3 C13 Cl2 113.6(2) . .
Cl2' C13 Cl3' 111.5(3) . .
Cl3 C13 Cl3' 8.0(3) . .
Cl2 C13 Cl3' 107.9(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag1 P1 2.4991(3) 2_655
Ag1 P1 2.4991(3) 3_665
Ag1 P1 2.4991(3) .
Ag1 B1 2.540(2) .
Ag1 Cl1 2.5797(6) .
P1 C2 1.8227(13) .
P1 C7 1.8547(13) .
P1 C10 1.8657(13) .
B1 C1 1.6051(13) 2_655
B1 C1 1.6051(13) 3_665
B1 C1 1.6051(13) .
C1 C6 1.4047(17) .
C1 C2 1.4078(17) .
C2 C3 1.4002(17) .
C3 C4 1.387(2) .
C4 C5 1.382(2) .
C5 C6 1.3856(19) .
C7 C8 1.529(2) .
C7 C9 1.5314(19) .
C10 C11 1.526(2) .
C10 C12 1.5338(19) .
C13 Cl2' 1.713(6) .
C13 Cl3 1.717(5) .
C13 Cl2 1.779(5) .
C13 Cl3' 1.784(5) .
