#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/71/2217190.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_2217190
loop_
_publ_author_name
'Chen, Yue'
'Zhou, Jin'
'Li, Xiaoyan'
_publ_section_title
cis-Dichlorido(3-chloro-2-methyliminophenyl-κ²C¹,N)-trans-bis(trimethylphosphine-κP)cobalt(III)
_journal_coeditor_code           LN2014
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m210
_journal_page_last               m210
_journal_paper_doi               10.1107/S1600536807062654
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Co Cl2 (C8 H7 Cl N) (C3 H9 P)2]'
_chemical_formula_moiety         'C14 H25 Cl3 Co N P2'
_chemical_formula_sum            'C14 H25 Cl3 Co N P2'
_chemical_formula_weight         434.57
_chemical_name_systematic
;
cis-Dichlorido(3-chloro-2-methyliminophenyl-κ²C¹,N)-trans-
bis(trimethylphosphine-\kP)cobalt(III)
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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            4
_cell_length_a                   8.5530(17)
_cell_length_b                   10.543(2)
_cell_length_c                   21.769(4)
_cell_measurement_reflns_used    3063
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      20.357
_cell_measurement_theta_min      3.088
_cell_volume                     1963.0(6)
_computing_cell_refinement       'SAINT (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2001)'
_computing_publication_material  'SHELXTL (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '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  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0242
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            16045
_diffrn_reflns_theta_full        28.46
_diffrn_reflns_theta_max         28.46
_diffrn_reflns_theta_min         1.87
_diffrn_standards_decay_%        0.02
_diffrn_standards_interval_count 5
_diffrn_standards_number         2699
_exptl_absorpt_coefficient_mu    1.439
_exptl_absorpt_correction_T_max  0.6888
_exptl_absorpt_correction_T_min  0.6721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.426
_refine_ls_abs_structure_details 'Flack (1983), 2082 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.001(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         4910
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0246
_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)+(0.0416P)²+0.7929P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0658
_reflns_number_gt                4868
_reflns_number_total             4910
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ln2014.cif
_cod_data_source_block           I
_cod_original_cell_volume        1963.0(7)
_cod_database_code               2217190
_cod_database_fobs_code          2217190
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'
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
N N1 0.03793(18) 0.45205(14) 0.18750(6) 0.0120(3) Uani d . 1
Co Co1 0.21282(3) 0.51827(2) 0.141359(10) 0.00967(6) Uani d . 1
Cl Cl1 0.41880(5) 0.58705(4) 0.08431(2) 0.01627(9) Uani d . 1
Cl Cl2 0.23616(5) 0.69589(4) 0.205711(19) 0.01659(9) Uani d . 1
Cl Cl3 -0.14169(5) 0.09058(4) 0.112040(19) 0.01852(9) Uani d . 1
P P1 0.06006(6) 0.62472(4) 0.07525(2) 0.01346(9) Uani d . 1
P P2 0.38816(5) 0.41085(4) 0.19781(2) 0.01276(9) Uani d . 1
C C1 0.1815(2) 0.36764(16) 0.09372(8) 0.0121(3) Uani d . 1
C C2 0.2656(2) 0.32345(17) 0.04297(8) 0.0159(3) Uani d . 1
H H2A 0.3464 0.3721 0.0268 0.019 Uiso calc R 1
C C3 0.2291(2) 0.20742(17) 0.01664(8) 0.0170(3) Uani d . 1
H H3A 0.2881 0.1787 -0.0164 0.020 Uiso calc R 1
C C4 0.1063(2) 0.13253(16) 0.03839(8) 0.0161(3) Uani d . 1
H H4A 0.0832 0.0549 0.0202 0.019 Uiso calc R 1
C C5 0.0203(2) 0.17679(16) 0.08749(8) 0.0136(3) Uani d . 1
C C6 0.0574(2) 0.29240(15) 0.11584(8) 0.0122(3) Uani d . 1
C C7 -0.0181(2) 0.34538(16) 0.16892(8) 0.0129(3) Uani d . 1
H H7A -0.1015 0.3055 0.1884 0.015 Uiso calc R 1
C C8 -0.0316(2) 0.50993(18) 0.24222(8) 0.0174(3) Uani d . 1
H H8A -0.1168 0.4584 0.2564 0.026 Uiso calc R 1
H H8B -0.0696 0.5931 0.2322 0.026 Uiso calc R 1
H H8C 0.0460 0.5163 0.2739 0.026 Uiso calc R 1
C C9 0.0955(3) 0.79342(18) 0.07302(10) 0.0258(4) Uani d . 1
H H9A 0.0261 0.8322 0.0439 0.039 Uiso calc R 1
H H9B 0.2018 0.8089 0.0610 0.039 Uiso calc R 1
H H9C 0.0774 0.8290 0.1130 0.039 Uiso calc R 1
C C10 0.0760(3) 0.5799(2) -0.00478(8) 0.0227(4) Uani d . 1
H H10A 0.0061 0.6308 -0.0289 0.034 Uiso calc R 1
H H10B 0.0489 0.4920 -0.0093 0.034 Uiso calc R 1
H H10C 0.1814 0.5930 -0.0185 0.034 Uiso calc R 1
C C11 -0.1493(2) 0.6155(2) 0.08898(10) 0.0258(4) Uani d . 1
H H11A -0.2035 0.6640 0.0583 0.039 Uiso calc R 1
H H11B -0.1726 0.6492 0.1289 0.039 Uiso calc R 1
H H11C -0.1824 0.5286 0.0869 0.039 Uiso calc R 1
C C12 0.3113(3) 0.3308(2) 0.26513(9) 0.0243(4) Uani d . 1
H H12A 0.3947 0.2879 0.2861 0.036 Uiso calc R 1
H H12B 0.2337 0.2702 0.2528 0.036 Uiso calc R 1
H H12C 0.2648 0.3920 0.2922 0.036 Uiso calc R 1
C C13 0.5434(3) 0.5051(2) 0.23006(12) 0.0293(5) Uani d . 1
H H13A 0.6122 0.4516 0.2533 0.044 Uiso calc R 1
H H13B 0.4998 0.5688 0.2565 0.044 Uiso calc R 1
H H13C 0.6009 0.5452 0.1976 0.044 Uiso calc R 1
C C14 0.4966(3) 0.2879(2) 0.15854(10) 0.0260(4) Uani d . 1
H H14A 0.5677 0.2484 0.1868 0.039 Uiso calc R 1
H H14B 0.5543 0.3246 0.1252 0.039 Uiso calc R 1
H H14C 0.4252 0.2256 0.1428 0.039 Uiso calc R 1
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'
N N 0.0061 0.0033 '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'
Co Co 0.3494 0.9721 '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
C7 N1 C8 117.90(15)
C7 N1 Co1 116.15(12)
C8 N1 Co1 125.91(12)
C1 Co1 N1 82.74(7)
C1 Co1 P1 89.20(5)
N1 Co1 P1 93.63(5)
C1 Co1 P2 88.36(5)
N1 Co1 P2 92.88(5)
P1 Co1 P2 172.71(2)
C1 Co1 Cl1 94.41(5)
N1 Co1 Cl1 177.13(5)
P1 Co1 Cl1 86.64(2)
P2 Co1 Cl1 86.69(2)
C1 Co1 Cl2 175.19(5)
N1 Co1 Cl2 92.52(5)
P1 Co1 Cl2 91.91(2)
P2 Co1 Cl2 91.09(2)
Cl1 Co1 Cl2 90.33(2)
C9 P1 C10 102.64(10)
C9 P1 C11 102.83(11)
C10 P1 C11 102.61(10)
C9 P1 Co1 114.36(7)
C10 P1 Co1 116.27(7)
C11 P1 Co1 116.19(7)
C13 P2 C14 101.64(11)
C13 P2 C12 102.05(11)
C14 P2 C12 103.56(11)
C13 P2 Co1 115.30(7)
C14 P2 Co1 116.43(7)
C12 P2 Co1 115.76(7)
C2 C1 C6 118.00(15)
C2 C1 Co1 129.22(13)
C6 C1 Co1 112.76(12)
C3 C2 C1 120.33(17)
C3 C2 H2A 119.8
C1 C2 H2A 119.8
C2 C3 C4 121.86(17)
C2 C3 H3A 119.1
C4 C3 H3A 119.1
C5 C4 C3 118.20(16)
C5 C4 H4A 120.9
C3 C4 H4A 120.9
C4 C5 C6 120.97(16)
C4 C5 Cl3 119.07(13)
C6 C5 Cl3 119.90(14)
C5 C6 C1 120.59(16)
C5 C6 C7 126.16(16)
C1 C6 C7 113.23(15)
N1 C7 C6 115.12(16)
N1 C7 H7A 122.4
C6 C7 H7A 122.4
N1 C8 H8A 109.5
N1 C8 H8B 109.5
H8A C8 H8B 109.5
N1 C8 H8C 109.5
H8A C8 H8C 109.5
H8B C8 H8C 109.5
P1 C9 H9A 109.5
P1 C9 H9B 109.5
H9A C9 H9B 109.5
P1 C9 H9C 109.5
H9A C9 H9C 109.5
H9B C9 H9C 109.5
P1 C10 H10A 109.5
P1 C10 H10B 109.5
H10A C10 H10B 109.5
P1 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
P2 C12 H12A 109.5
P2 C12 H12B 109.5
H12A C12 H12B 109.5
P2 C12 H12C 109.5
H12A C12 H12C 109.5
H12B C12 H12C 109.5
P2 C13 H13A 109.5
P2 C13 H13B 109.5
H13A C13 H13B 109.5
P2 C13 H13C 109.5
H13A C13 H13C 109.5
H13B C13 H13C 109.5
P2 C14 H14A 109.5
P2 C14 H14B 109.5
H14A C14 H14B 109.5
P2 C14 H14C 109.5
H14A C14 H14C 109.5
H14B C14 H14C 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
N1 C7 1.288(2)
N1 C8 1.465(2)
N1 Co1 1.9323(15)
Co1 C1 1.9155(17)
Co1 P1 2.2444(6)
Co1 P2 2.2455(5)
Co1 Cl1 2.2742(5)
Co1 Cl2 2.3471(6)
Cl3 C5 1.7411(18)
P1 C9 1.805(2)
P1 C10 1.8105(19)
P1 C11 1.818(2)
P2 C13 1.801(2)
P2 C14 1.808(2)
P2 C12 1.814(2)
C1 C2 1.398(2)
C1 C6 1.410(2)
C2 C3 1.386(2)
C2 H2A 0.9300
C3 C4 1.397(3)
C3 H3A 0.9300
C4 C5 1.379(3)
C4 H4A 0.9300
C5 C6 1.403(2)
C6 C7 1.437(2)
C7 H7A 0.9300
C8 H8A 0.9600
C8 H8B 0.9600
C8 H8C 0.9600
C9 H9A 0.9600
C9 H9B 0.9600
C9 H9C 0.9600
C10 H10A 0.9600
C10 H10B 0.9600
C10 H10C 0.9600
C11 H11A 0.9600
C11 H11B 0.9600
C11 H11C 0.9600
C12 H12A 0.9600
C12 H12B 0.9600
C12 H12C 0.9600
C13 H13A 0.9600
C13 H13B 0.9600
C13 H13C 0.9600
C14 H14A 0.9600
C14 H14B 0.9600
C14 H14C 0.9600
