#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:14:32 +0100 (vie 25 de mar de 2016) $
#$Revision: 179805 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/01/7010150.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_7010150
loop_
_publ_author_name
'Lu, Norman'
'Norman, Nicholas C.'
'Orpen, A. Guy'
'Quayle, Michael J.'
'Timms, Peter L.'
'Whittell, George R.'
_publ_section_title
;
 Transition metal complexes incorporating the BF2 ligand formed by
 oxidative addition of the B--B bond in B2F4
;
_journal_issue                   22
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4032
_journal_paper_doi               10.1039/b006535h
_journal_year                    2000
_chemical_formula_sum            'C6.86 H20.57 B0.57 Co0.57 F2.29 P2.29'
_chemical_formula_weight         257.16
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           198
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P 21 3'
_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                90.00
_cell_formula_units_Z            7
_cell_length_a                   13.2859(6)
_cell_length_b                   13.2859(6)
_cell_length_c                   13.2859(6)
_cell_measurement_reflns_used    87
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      50
_cell_measurement_theta_min      5
_cell_volume                     2345.16(18)
_computing_cell_refinement       'SAINT (Siemens, 1995b)'
_computing_data_collection       'SMART (Siemens, 1995b)'
_computing_data_reduction        'SAINT (Siemens, 1995b)'
_computing_molecular_graphics    'SHELXTL (Siemens, 1995a)'
_computing_publication_material  'SHELXTL (Siemens, 1995a)'
_computing_structure_refinement  'SHELXTL (Siemens, 1995a)'
_computing_structure_solution    'SHELXTL (Siemens, 1995a)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Siemens SMART Area Detector'
_diffrn_measurement_method       'ω rotation with narrow frame'
_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  0.0459
_diffrn_reflns_av_sigmaI/netI    0.0269
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15447
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    1.027
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.772
_exptl_absorpt_correction_type   'SADABS (Sheldrick, 1996)'
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             944
_refine_diff_density_max         0.234
_refine_diff_density_min         -0.161
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     84
_refine_ls_number_reflns         1814
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0311
_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)+(0.0444P)²+0.0000P] whereP=(Max(Fo²,0)+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0728
_reflns_number_gt                1459
_reflns_number_total             1814
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b006535h.txt
_cod_data_source_block           '[Co(PMe3)4][BF4]'
_cod_original_sg_symbol_H-M      P2(1)3
_cod_database_code               7010150
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
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
Co1 Co 0.20846(2) 0.20846(2) 0.20846(2) 0.04590(15) Uani 1 3 d S . .
P1 P 0.27485(5) 0.05759(5) 0.17676(5) 0.05242(18) Uani 1 1 d . . .
C3 C 0.2127(3) -0.0257(2) 0.0859(2) 0.0735(8) Uani 1 1 d . . .
H3A H 0.1436 -0.0349 0.1049 0.110 Uiso 1 1 calc R . .
H3B H 0.2462 -0.0897 0.0851 0.110 Uiso 1 1 calc R . .
H3C H 0.2158 0.0039 0.0200 0.110 Uiso 1 1 calc R . .
C2 C 0.2896(4) -0.0280(3) 0.2831(2) 0.1159(16) Uani 1 1 d . . .
H2A H 0.2258 -0.0371 0.3158 0.174 Uiso 1 1 calc R . .
H2B H 0.3370 -0.0002 0.3301 0.174 Uiso 1 1 calc R . .
H2C H 0.3138 -0.0919 0.2595 0.174 Uiso 1 1 calc R . .
C1 C 0.4016(2) 0.0574(3) 0.1251(3) 0.0841(10) Uani 1 1 d . . .
H1A H 0.4468 0.0887 0.1720 0.126 Uiso 1 1 calc R . .
H1B H 0.4023 0.0942 0.0629 0.126 Uiso 1 1 calc R . .
H1C H 0.4226 -0.0106 0.1130 0.126 Uiso 1 1 calc R . .
P2 P 0.30562(5) 0.30562(5) 0.30562(5) 0.0631(3) Uani 1 3 d S . .
C4 C 0.4195(3) 0.3541(4) 0.2481(4) 0.1181(16) Uani 1 1 d . . .
H4A H 0.4022 0.3952 0.1913 0.177 Uiso 1 1 calc R . .
H4B H 0.4609 0.2990 0.2264 0.177 Uiso 1 1 calc R . .
H4C H 0.4558 0.3939 0.2964 0.177 Uiso 1 1 calc R . .
B1 B 0.3428(3) -0.3428(3) 0.1572(3) 0.0754(17) Uani 1 3 d S . .
F1 F 0.3818(6) -0.3456(5) 0.2475(4) 0.152(3) Uani 0.726(14) 1 d P A 1
F2 F 0.4013(3) -0.4013(3) 0.0987(3) 0.195(6) Uani 0.726(14) 3 d SP A 1
F2' F 0.2806(8) -0.2806(8) 0.2194(8) 0.207(16) Uani 0.274(14) 3 d SP A 2
F3 F 0.2851(17) -0.4121(12) 0.1277(12) 0.209(13) Uani 0.274(14) 1 d P A 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'
F F 0.0171 0.0103 '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'
Co Co 0.3494 0.9721 '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'
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
_geom_angle_publ_flag
P1 Co1 P1 105.09(2) . 5 ?
P1 Co1 P1 105.09(2) . 9 ?
P1 Co1 P1 105.09(2) 5 9 ?
P1 Co1 P2 113.56(2) . . ?
P1 Co1 P2 113.56(2) 5 . ?
P1 Co1 P2 113.56(2) 9 . ?
C1 P1 C2 101.1(2) . . ?
C1 P1 C3 99.64(16) . . ?
C2 P1 C3 100.49(18) . . ?
C1 P1 Co1 116.01(12) . . ?
C2 P1 Co1 117.17(11) . . ?
C3 P1 Co1 119.26(10) . . ?
C4 P2 C4 101.79(17) 5 9 ?
C4 P2 C4 101.79(17) 5 . ?
C4 P2 C4 101.79(17) 9 . ?
C4 P2 Co1 116.36(14) 5 . ?
C4 P2 Co1 116.36(14) 9 . ?
C4 P2 Co1 116.36(14) . . ?
F3 B1 F3 113.9(10) 7 10_545 ?
F3 B1 F3 113.9(10) 7 . ?
F3 B1 F3 113.9(10) 10_545 . ?
F3 B1 F1 31.1(12) 7 10_545 ?
F3 B1 F1 120.4(10) 10_545 10_545 ?
F3 B1 F1 124.4(10) . 10_545 ?
F3 B1 F1 120.4(10) 7 7 ?
F3 B1 F1 124.4(10) 10_545 7 ?
F3 B1 F1 31.1(12) . 7 ?
F1 B1 F1 112.3(4) 10_545 7 ?
F3 B1 F1 124.4(10) 7 . ?
F3 B1 F1 31.1(12) 10_545 . ?
F3 B1 F1 120.4(10) . . ?
F1 B1 F1 112.3(4) 10_545 . ?
F1 B1 F1 112.3(4) 7 . ?
F3 B1 F2 75.5(12) 7 . ?
F3 B1 F2 75.5(12) 10_545 . ?
F3 B1 F2 75.5(12) . . ?
F1 B1 F2 106.5(5) 10_545 . ?
F1 B1 F2 106.5(5) 7 . ?
F1 B1 F2 106.5(5) . . ?
F3 B1 F2' 104.5(12) 7 . ?
F3 B1 F2' 104.5(12) 10_545 . ?
F3 B1 F2' 104.5(12) . . ?
F1 B1 F2' 73.5(5) 10_545 . ?
F1 B1 F2' 73.5(5) 7 . ?
F1 B1 F2' 73.5(5) . . ?
F2 B1 F2' 180.0(14) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 P1 2.2300(7) . ?
Co1 P1 2.2300(7) 5 ?
Co1 P1 2.2301(7) 9 ?
Co1 P2 2.2357(13) . ?
P1 C1 1.819(3) . ?
P1 C2 1.825(3) . ?
P1 C3 1.834(3) . ?
P2 C4 1.814(4) 5 ?
P2 C4 1.814(4) 9 ?
P2 C4 1.814(4) . ?
B1 F3 1.260(12) 7 ?
B1 F3 1.260(12) 10_545 ?
B1 F3 1.260(12) . ?
B1 F1 1.308(5) 10_545 ?
B1 F1 1.308(5) 7 ?
B1 F1 1.308(5) . ?
B1 F2 1.347(11) . ?
B1 F2' 1.431(19) . ?
