#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/58/2225846.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2225846
loop_
_publ_author_name
'Zheng, Tingting'
'Sun, Hongjian'
_publ_section_title
;
 Dichlorido[2,3,5,6-tetrafluoro-4-(trifluoromethyl)phenyl-κC¹]bis(trimethylphosphine-κP)cobalt(III)
;
_journal_coeditor_code           GK2264
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m574
_journal_paper_doi               10.1107/S1600536810014066
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Co (C7 F7) Cl2 (C3 H9 P)2]'
_chemical_formula_moiety         'C13 H18 Cl2 Co F7 P2'
_chemical_formula_sum            'C13 H18 Cl2 Co F7 P2'
_chemical_formula_weight         499.04
_chemical_melting_point          380
_chemical_name_systematic
;
Dichlorido[2,3,5,6-tetrafluoro-4-(trifluoromethyl)phenyl-
κC¹]bis(trimethylphosphine-κP)cobalt(III)
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            8
_cell_length_a                   12.3321(19)
_cell_length_b                   13.3657(19)
_cell_length_c                   25.426(4)
_cell_measurement_reflns_used    2967
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.04
_cell_measurement_theta_min      2.30
_cell_volume                     4190.9(11)
_computing_cell_refinement       'SAINT (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'φ and ω 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  0.0522
_diffrn_reflns_av_sigmaI/netI    0.0378
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            18353
_diffrn_reflns_theta_full        24.23
_diffrn_reflns_theta_max         24.23
_diffrn_reflns_theta_min         2.30
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.280
_exptl_absorpt_correction_T_max  0.8023
_exptl_absorpt_correction_T_min  0.7402
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.778
_refine_diff_density_min         -0.692
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         3373
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0935P)²+7.5678P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1644
_refine_ls_wR_factor_ref         0.1860
_reflns_number_gt                2345
_reflns_number_total             3373
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            gk2264.cif
_cod_data_source_block           I
_cod_original_cell_volume        4190.8(11)
_cod_database_code               2225846
_cod_database_fobs_code          2225846
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'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.9572(5) 0.1013(5) 0.1322(3) 0.0593(16) Uani d . 1 A .
C C2 0.9141(7) 0.1728(6) 0.0990(3) 0.080(2) Uani d . 1 . .
C C3 0.8099(8) 0.1731(9) 0.0813(3) 0.102(3) Uani d . 1 A .
C C4 0.7378(6) 0.0992(11) 0.0944(4) 0.109(4) Uani d D 1 . .
C C5 0.7789(7) 0.0239(8) 0.1266(3) 0.094(3) Uani d . 1 A .
C C6 0.8834(6) 0.0266(6) 0.1449(3) 0.073(2) Uani d . 1 . .
C C8 1.3056(6) -0.0189(6) 0.0919(3) 0.087(2) Uani d . 1 . .
H H8A 1.3203 -0.0538 0.1241 0.130 Uiso calc R 1 . .
H H8B 1.3477 0.0414 0.0907 0.130 Uiso calc R 1 . .
H H8C 1.3244 -0.0607 0.0626 0.130 Uiso calc R 1 . .
C C9 1.1447(8) 0.0770(7) 0.0268(3) 0.101(3) Uani d . 1 . .
H H9A 1.1794 0.1413 0.0286 0.151 Uiso calc R 1 . .
H H9B 1.0687 0.0858 0.0201 0.151 Uiso calc R 1 . .
H H9C 1.1766 0.0384 -0.0010 0.151 Uiso calc R 1 . .
C C10 1.0943(7) -0.1069(5) 0.0800(3) 0.087(2) Uani d . 1 . .
H H10A 1.1015 -0.1461 0.1115 0.130 Uiso calc R 1 . .
H H10B 1.1264 -0.1422 0.0510 0.130 Uiso calc R 1 . .
H H10C 1.0189 -0.0954 0.0729 0.130 Uiso calc R 1 . .
C C11 1.1647(6) 0.2311(6) 0.2713(3) 0.092(3) Uani d . 1 . .
H H11A 1.2031 0.1723 0.2824 0.137 Uiso calc R 1 . .
H H11B 1.1369 0.2656 0.3016 0.137 Uiso calc R 1 . .
H H11C 1.2131 0.2744 0.2524 0.137 Uiso calc R 1 . .
C C12 0.9874(8) 0.3117(6) 0.2110(4) 0.105(3) Uani d . 1 . .
H H12A 1.0344 0.3495 0.1884 0.157 Uiso calc R 1 . .
H H12B 0.9727 0.3495 0.2423 0.157 Uiso calc R 1 . .
H H12C 0.9206 0.2979 0.1931 0.157 Uiso calc R 1 . .
C C13 0.9579(7) 0.1302(8) 0.2711(3) 0.101(3) Uani d . 1 . .
H H13A 0.9885 0.0672 0.2816 0.151 Uiso calc R 1 . .
H H13B 0.8913 0.1187 0.2525 0.151 Uiso calc R 1 . .
H H13C 0.9438 0.1701 0.3017 0.151 Uiso calc R 1 . .
Cl Cl1 1.22875(15) 0.22034(13) 0.13739(8) 0.0772(6) Uani d . 1 A .
Cl Cl2 1.18147(13) -0.01081(11) 0.21464(6) 0.0566(4) Uani d . 1 A .
Co Co1 1.10845(6) 0.10295(6) 0.15914(3) 0.0498(3) Uani d . 1 . .
F F1 0.9169(4) -0.0490(4) 0.17618(19) 0.0965(15) Uani d . 1 A .
F F2 0.7167(4) -0.0546(6) 0.1418(2) 0.146(3) Uani d . 1 . .
F F3 0.7792(5) 0.2497(5) 0.0496(2) 0.156(3) Uani d . 1 . .
F F4 0.9791(5) 0.2502(4) 0.0832(2) 0.1083(16) Uani d . 1 . .
P P1 1.05246(15) 0.19513(14) 0.22862(7) 0.0664(5) Uani d . 1 A .
P P2 1.16269(14) 0.01209(14) 0.08875(7) 0.0622(5) Uani d . 1 A .
C C7 0.6149(13) 0.0863(14) 0.0797(8) 0.106(9) Uiso d PD 0.487(13) A 1
F F6 0.5612(14) 0.0191(12) 0.1062(6) 0.154(7) Uiso d PD 0.487(13) A 1
F F5 0.5737(12) 0.1839(12) 0.0899(6) 0.138(6) Uiso d PD 0.487(13) A 1
F F7 0.6077(13) 0.0920(13) 0.0284(6) 0.150(6) Uiso d PD 0.487(13) A 1
C C7' 0.6232(14) 0.1080(15) 0.0695(8) 0.141(12) Uiso d PD 0.513(13) A 2
F F6' 0.6148(12) 0.1727(13) 0.0306(6) 0.158(6) Uiso d PD 0.513(13) A 2
F F7' 0.6005(11) 0.0140(10) 0.0511(5) 0.133(5) Uiso d PD 0.513(13) A 2
F F5' 0.5527(11) 0.1180(11) 0.1069(5) 0.131(5) Uiso d PD 0.513(13) 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'
Cl Cl 0.1484 0.1585 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 C1 C6 . . 112.8(7) ?
C2 C1 Co1 . . 124.3(6) ?
C6 C1 Co1 . . 122.9(5) ?
C3 C2 F4 . . 117.0(8) ?
C3 C2 C1 . . 124.5(9) ?
F4 C2 C1 . . 118.5(7) ?
F3 C3 C2 . . 117.5(11) ?
F3 C3 C4 . . 120.4(9) ?
C2 C3 C4 . . 122.1(9) ?
C3 C4 C5 . . 115.3(7) ?
C3 C4 C7' . . 115.9(12) ?
C5 C4 C7' . . 128.7(13) ?
C3 C4 C7 . . 130.4(12) ?
C5 C4 C7 . . 114.3(12) ?
C7' C4 C7 . . 14.8(11) ?
F2 C5 C6 . . 117.1(9) ?
F2 C5 C4 . . 121.3(8) ?
C6 C5 C4 . . 121.6(9) ?
F1 C6 C5 . . 118.0(8) ?
F1 C6 C1 . . 118.3(6) ?
C5 C6 C1 . . 123.8(8) ?
P2 C8 H8A . . 109.5 ?
P2 C8 H8B . . 109.5 ?
H8A C8 H8B . . 109.5 ?
P2 C8 H8C . . 109.5 ?
H8A C8 H8C . . 109.5 ?
H8B C8 H8C . . 109.5 ?
P2 C9 H9A . . 109.5 ?
P2 C9 H9B . . 109.5 ?
H9A C9 H9B . . 109.5 ?
P2 C9 H9C . . 109.5 ?
H9A C9 H9C . . 109.5 ?
H9B C9 H9C . . 109.5 ?
P2 C10 H10A . . 109.5 ?
P2 C10 H10B . . 109.5 ?
H10A C10 H10B . . 109.5 ?
P2 C10 H10C . . 109.5 ?
H10A C10 H10C . . 109.5 ?
H10B C10 H10C . . 109.5 ?
P1 C11 H11A . . 109.5 ?
P1 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
P1 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
P1 C12 H12A . . 109.5 ?
P1 C12 H12B . . 109.5 ?
H12A C12 H12B . . 109.5 ?
P1 C12 H12C . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
P1 C13 H13A . . 109.5 ?
P1 C13 H13B . . 109.5 ?
H13A C13 H13B . . 109.5 ?
P1 C13 H13C . . 109.5 ?
H13A C13 H13C . . 109.5 ?
H13B C13 H13C . . 109.5 ?
C1 Co1 Cl1 . . 123.2(2) y
C1 Co1 Cl2 . . 125.5(2) y
Cl1 Co1 Cl2 . . 111.29(7) y
C1 Co1 P1 . . 89.36(19) y
Cl1 Co1 P1 . . 90.78(8) y
Cl2 Co1 P1 . . 90.03(7) y
C1 Co1 P2 . . 89.93(19) y
Cl1 Co1 P2 . . 89.13(8) y
Cl2 Co1 P2 . . 90.86(7) y
P1 Co1 P2 . . 179.08(8) y
C12 P1 C13 . . 105.9(5) ?
C12 P1 C11 . . 104.9(4) ?
C13 P1 C11 . . 105.1(4) ?
C12 P1 Co1 . . 114.3(3) ?
C13 P1 Co1 . . 113.6(3) ?
C11 P1 Co1 . . 112.1(3) ?
C9 P2 C8 . . 105.5(4) ?
C9 P2 C10 . . 104.9(4) ?
C8 P2 C10 . . 104.9(4) ?
C9 P2 Co1 . . 113.2(3) ?
C8 P2 Co1 . . 112.0(3) ?
C10 P2 Co1 . . 115.5(3) ?
F6 C7 F7 . . 121.3(17) ?
F6 C7 F5 . . 110.9(16) ?
F7 C7 F5 . . 96.0(15) ?
F6 C7 C4 . . 116.3(16) ?
F7 C7 C4 . . 107.2(14) ?
F5 C7 C4 . . 101.6(13) ?
F5' C7' F6' . . 115.5(17) ?
F5' C7' F7' . . 102.1(16) ?
F6' C7' F7' . . 109.3(16) ?
F5' C7' C4 . . 108.5(15) ?
F6' C7' C4 . . 115.3(16) ?
F7' C7' C4 . . 104.8(14) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C2 . 1.382(10) ?
C1 C6 . 1.389(10) ?
C1 Co1 . 1.987(6) y
C2 C3 . 1.362(12) ?
C2 F4 . 1.369(9) ?
C3 F3 . 1.358(11) ?
C3 C4 . 1.370(15) ?
C4 C5 . 1.393(14) ?
C4 C7' . 1.554(17) ?
C4 C7 . 1.570(16) ?
C5 F2 . 1.357(11) ?
C5 C6 . 1.370(11) ?
C6 F1 . 1.350(9) ?
C8 P2 . 1.812(7) ?
C8 H8A . 0.9600 ?
C8 H8B . 0.9600 ?
C8 H8C . 0.9600 ?
C9 P2 . 1.812(8) ?
C9 H9A . 0.9600 ?
C9 H9B . 0.9600 ?
C9 H9C . 0.9600 ?
C10 P2 . 1.814(8) ?
C10 H10A . 0.9600 ?
C10 H10B . 0.9600 ?
C10 H10C . 0.9600 ?
C11 P1 . 1.823(8) ?
C11 H11A . 0.9600 ?
C11 H11B . 0.9600 ?
C11 H11C . 0.9600 ?
C12 P1 . 1.808(8) ?
C12 H12A . 0.9600 ?
C12 H12B . 0.9600 ?
C12 H12C . 0.9600 ?
C13 P1 . 1.811(8) ?
C13 H13A . 0.9600 ?
C13 H13B . 0.9600 ?
C13 H13C . 0.9600 ?
Cl1 Co1 . 2.2290(18) y
Cl2 Co1 . 2.2613(16) y
Co1 P1 . 2.262(2) y
Co1 P2 . 2.264(2) y
C7 F6 . 1.302(16) ?
C7 F7 . 1.311(17) ?
C7 F5 . 1.424(17) ?
C7' F5' . 1.296(17) ?
C7' F6' . 1.317(17) ?
C7' F7' . 1.368(17) ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C6 C1 C2 C3 . . . . 1.7(11) ?
Co1 C1 C2 C3 . . . . -178.6(6) ?
C6 C1 C2 F4 . . . . -179.5(7) ?
Co1 C1 C2 F4 . . . . 0.2(10) ?
F4 C2 C3 F3 . . . . 0.1(12) ?
C1 C2 C3 F3 . . . . 178.9(7) ?
F4 C2 C3 C4 . . . . 179.7(8) ?
C1 C2 C3 C4 . . . . -1.5(14) ?
F3 C3 C4 C5 . . . . 179.1(7) ?
C2 C3 C4 C5 . . . . -0.4(13) ?
F3 C3 C4 C7' . . . . 1.8(15) ?
C2 C3 C4 C7' . . . . -177.8(11) ?
F3 C3 C4 C7 . . . . -2.0(17) ?
C2 C3 C4 C7 . . . . 178.5(12) ?
C3 C4 C5 F2 . . . . -178.9(8) ?
C7' C4 C5 F2 . . . . -1.9(16) ?
C7 C4 C5 F2 . . . . 2.0(14) ?
C3 C4 C5 C6 . . . . 2.0(13) ?
C7' C4 C5 C6 . . . . 179.0(12) ?
C7 C4 C5 C6 . . . . -177.1(10) ?
F2 C5 C6 F1 . . . . 0.5(11) ?
C4 C5 C6 F1 . . . . 179.6(7) ?
F2 C5 C6 C1 . . . . 179.0(7) ?
C4 C5 C6 C1 . . . . -1.8(13) ?
C2 C1 C6 F1 . . . . 178.4(7) ?
Co1 C1 C6 F1 . . . . -1.3(10) ?
C2 C1 C6 C5 . . . . -0.1(11) ?
Co1 C1 C6 C5 . . . . -179.8(6) ?
C2 C1 Co1 Cl1 . . . . -1.3(7) ?
C6 C1 Co1 Cl1 . . . . 178.4(5) ?
C2 C1 Co1 Cl2 . . . . 178.8(5) ?
C6 C1 Co1 Cl2 . . . . -1.5(7) ?
C2 C1 Co1 P1 . . . . 89.2(6) ?
C6 C1 Co1 P1 . . . . -91.1(6) ?
C2 C1 Co1 P2 . . . . -90.2(6) ?
C6 C1 Co1 P2 . . . . 89.5(6) ?
C1 Co1 P1 C12 . . . . -57.7(4) ?
Cl1 Co1 P1 C12 . . . . 65.5(4) ?
Cl2 Co1 P1 C12 . . . . 176.8(4) ?
C1 Co1 P1 C13 . . . . 64.1(4) ?
Cl1 Co1 P1 C13 . . . . -172.7(3) ?
Cl2 Co1 P1 C13 . . . . -61.4(3) ?
C1 Co1 P1 C11 . . . . -176.9(4) ?
Cl1 Co1 P1 C11 . . . . -53.7(3) ?
Cl2 Co1 P1 C11 . . . . 57.6(3) ?
C1 Co1 P2 C9 . . . . 63.6(4) ?
Cl1 Co1 P2 C9 . . . . -59.6(4) ?
Cl2 Co1 P2 C9 . . . . -170.8(4) ?
C1 Co1 P2 C8 . . . . -177.3(4) ?
Cl1 Co1 P2 C8 . . . . 59.6(3) ?
Cl2 Co1 P2 C8 . . . . -51.7(3) ?
C1 Co1 P2 C10 . . . . -57.3(3) ?
Cl1 Co1 P2 C10 . . . . 179.5(3) ?
Cl2 Co1 P2 C10 . . . . 68.2(3) ?
C3 C4 C7 F6 . . . . -166.9(13) ?
C5 C4 C7 F6 . . . . 12.0(19) ?
C7' C4 C7 F6 . . . . 180(5) ?
C3 C4 C7 F7 . . . . 54(2) ?
C5 C4 C7 F7 . . . . -127.5(14) ?
C7' C4 C7 F7 . . . . 40(4) ?
C3 C4 C7 F5 . . . . -46.5(19) ?
C5 C4 C7 F5 . . . . 132.4(12) ?
C7' C4 C7 F5 . . . . -60(4) ?
C3 C4 C7' F5' . . . . -118.0(15) ?
C5 C4 C7' F5' . . . . 65(2) ?
C7 C4 C7' F5' . . . . 51(4) ?
C3 C4 C7' F6' . . . . 13(2) ?
C5 C4 C7' F6' . . . . -163.6(13) ?
C7 C4 C7' F6' . . . . -178(5) ?
C3 C4 C7' F7' . . . . 133.6(13) ?
C5 C4 C7' F7' . . . . -43.3(19) ?
C7 C4 C7' F7' . . . . -58(4) ?
