#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:31:10 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179752 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/48/7004854.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_7004854
loop_
_publ_author_name
'Suzuki, Takayoshi'
'Fujiiwara, Katsuhiro'
'Takagi, Hideo D.'
'Kashiwabara, Kazuo'
_publ_section_title
;
 Preparation and characterization of mixed-ligand cobalt(III) complexes
 containing (3-aminopropyl)dimethylphosphine (pdmp). Conformation of
 the six-membered pdmp chelate ring.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              308
_journal_page_last               319
_journal_paper_doi               10.1039/b612025c
_journal_year                    2007
_chemical_formula_moiety         'C10 H28 Cl2 Co N2 P2 1+, F6 P 1-'
_chemical_formula_sum            'C10 H28 Cl2 Co F6 N2 P3'
_chemical_formula_weight         513.08
_chemical_name_common
;
trans(Cl,Cl)cis(P,P)-dichlorobis((3-
aminopropyl)dimethylphosphine)cobalt(iii) hexafluorophosphate
;
_chemical_name_systematic
;
trans(Cl,Cl)cis(P,P)-dichlorobis((3-aminopropyl)dimethylphosphine)cobalt(III)
hexafluorophosphate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                105.659(12)
_cell_angle_beta                 94.09(2)
_cell_angle_gamma                98.15(2)
_cell_formula_units_Z            2
_cell_length_a                   8.178(11)
_cell_length_b                   10.073(13)
_cell_length_c                   12.811(16)
_cell_measurement_reflns_used    3077
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     999(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        'CrystalStructure 3.7.0'
_computing_molecular_graphics    'ORTEP3 for win'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0519
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7883
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    1.416
_exptl_absorpt_correction_T_max  0.9325
_exptl_absorpt_correction_T_min  0.7648
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         4364
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0421
_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)+(0.0430P)²+0.3128P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.0985
_reflns_number_gt                3617
_reflns_number_total             4364
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            b612025c.txt
_cod_data_source_block           pdmpCl2P
_cod_database_code               7004854
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 -0.01482(4) 0.83736(4) 0.74476(3) 0.01582(11) Uani 1 1 d . . .
Cl1 Cl 0.14064(9) 0.73548(8) 0.61793(6) 0.02578(17) Uani 1 1 d . . .
Cl2 Cl -0.17103(9) 0.94521(7) 0.86758(5) 0.02531(17) Uani 1 1 d . . .
P1 P -0.25405(9) 0.74350(7) 0.63949(6) 0.01928(16) Uani 1 1 d . . .
P2 P -0.00244(9) 0.65719(8) 0.81232(6) 0.02312(17) Uani 1 1 d . . .
P3 P 0.44222(10) 0.27158(8) 0.77718(7) 0.02595(18) Uani 1 1 d . . .
F1 F 0.2634(3) 0.2904(3) 0.7299(2) 0.0575(6) Uani 1 1 d . . .
F2 F 0.3920(3) 0.1073(2) 0.71727(18) 0.0480(5) Uani 1 1 d . . .
F3 F 0.5173(3) 0.2916(2) 0.66967(17) 0.0471(5) Uani 1 1 d . . .
F4 F 0.3642(3) 0.2474(2) 0.88247(17) 0.0493(6) Uani 1 1 d . . .
F5 F 0.4862(3) 0.4341(2) 0.83434(19) 0.0538(6) Uani 1 1 d . . .
F6 F 0.6173(3) 0.2495(3) 0.82239(19) 0.0575(6) Uani 1 1 d . . .
N1 N 0.0086(3) 0.9987(3) 0.6744(2) 0.0270(6) Uani 1 1 d . . .
H1A H 0.0922 1.0656 0.7182 0.032 Uiso 1 1 calc R . .
H1B H 0.0504 0.9645 0.6095 0.032 Uiso 1 1 calc R . .
N2 N 0.1865(3) 0.9453(2) 0.85406(18) 0.0216(5) Uani 1 1 d . . .
H2A H 0.2146 1.0290 0.8384 0.026 Uiso 1 1 calc R . .
H2B H 0.1485 0.9665 0.9215 0.026 Uiso 1 1 calc R . .
C1 C -0.4123(4) 0.6491(3) 0.6956(3) 0.0320(7) Uani 1 1 d . . .
H1C H -0.4260 0.7056 0.7687 0.038 Uiso 1 1 calc R . .
H1D H -0.3791 0.5608 0.7001 0.038 Uiso 1 1 calc R . .
H1E H -0.5177 0.6294 0.6484 0.038 Uiso 1 1 calc R . .
C2 C -0.2426(4) 0.6273(3) 0.5063(2) 0.0331(7) Uani 1 1 d . . .
H2C H -0.1584 0.6715 0.4699 0.040 Uiso 1 1 calc R . .
H2D H -0.3510 0.6078 0.4624 0.040 Uiso 1 1 calc R . .
H2E H -0.2124 0.5395 0.5143 0.040 Uiso 1 1 calc R . .
C3 C -0.3625(4) 0.8772(3) 0.6101(3) 0.0269(6) Uani 1 1 d . . .
H3A H -0.4608 0.8304 0.5564 0.032 Uiso 1 1 calc R . .
H3B H -0.4037 0.9279 0.6779 0.032 Uiso 1 1 calc R . .
C4 C -0.2604(4) 0.9832(3) 0.5661(3) 0.0330(7) Uani 1 1 d . . .
H4A H -0.2122 0.9332 0.5011 0.040 Uiso 1 1 calc R . .
H4B H -0.3344 1.0422 0.5427 0.040 Uiso 1 1 calc R . .
C5 C -0.1218(4) 1.0761(3) 0.6488(3) 0.0293(7) Uani 1 1 d . . .
H5A H -0.0715 1.1524 0.6201 0.035 Uiso 1 1 calc R . .
H5B H -0.1685 1.1190 0.7167 0.035 Uiso 1 1 calc R . .
C6 C -0.0747(4) 0.4815(3) 0.7231(3) 0.0384(8) Uani 1 1 d . . .
H6A H -0.0252 0.4706 0.6544 0.046 Uiso 1 1 calc R . .
H6B H -0.1961 0.4659 0.7080 0.046 Uiso 1 1 calc R . .
H6C H -0.0417 0.4131 0.7588 0.046 Uiso 1 1 calc R . .
C7 C -0.1012(5) 0.6642(4) 0.9357(3) 0.0426(9) Uani 1 1 d . . .
H7A H -0.0672 0.7572 0.9876 0.051 Uiso 1 1 calc R . .
H7B H -0.0674 0.5934 0.9684 0.051 Uiso 1 1 calc R . .
H7C H -0.2223 0.6459 0.9177 0.051 Uiso 1 1 calc R . .
C8 C 0.2125(4) 0.6439(3) 0.8513(3) 0.0299(7) Uani 1 1 d . . .
H8A H 0.2111 0.5714 0.8904 0.036 Uiso 1 1 calc R . .
H8B H 0.2649 0.6108 0.7838 0.036 Uiso 1 1 calc R . .
C9 C 0.3227(4) 0.7777(4) 0.9229(3) 0.0342(7) Uani 1 1 d . . .
H9A H 0.2730 0.8107 0.9915 0.041 Uiso 1 1 calc R . .
H9B H 0.4333 0.7560 0.9421 0.041 Uiso 1 1 calc R . .
C10 C 0.3444(4) 0.8929(3) 0.8685(3) 0.0280(7) Uani 1 1 d . . .
H10A H 0.4301 0.9707 0.9135 0.034 Uiso 1 1 calc R . .
H10B H 0.3836 0.8575 0.7964 0.034 Uiso 1 1 calc R . .
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'
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'
P P 0.1023 0.0942 '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'
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
N2 Co1 N1 87.95(12) . . ?
N2 Co1 P2 88.33(10) . . ?
N1 Co1 P2 171.18(8) . . ?
N2 Co1 P1 171.57(7) . . ?
N1 Co1 P1 89.58(9) . . ?
P2 Co1 P1 95.20(7) . . ?
N2 Co1 Cl2 86.32(12) . . ?
N1 Co1 Cl2 92.01(11) . . ?
P2 Co1 Cl2 95.74(8) . . ?
P1 Co1 Cl2 85.71(10) . . ?
N2 Co1 Cl1 94.05(12) . . ?
N1 Co1 Cl1 85.77(11) . . ?
P2 Co1 Cl1 86.52(8) . . ?
P1 Co1 Cl1 93.80(10) . . ?
Cl2 Co1 Cl1 177.73(3) . . ?
C1 P1 C2 104.37(18) . . ?
C1 P1 C3 100.98(17) . . ?
C2 P1 C3 103.83(17) . . ?
C1 P1 Co1 117.27(14) . . ?
C2 P1 Co1 116.96(12) . . ?
C3 P1 Co1 111.46(13) . . ?
C7 P2 C6 105.36(19) . . ?
C7 P2 C8 103.86(17) . . ?
C6 P2 C8 100.09(16) . . ?
C7 P2 Co1 115.63(12) . . ?
C6 P2 Co1 118.62(15) . . ?
C8 P2 Co1 111.25(11) . . ?
F6 P3 F5 91.08(15) . . ?
F6 P3 F4 90.95(14) . . ?
F5 P3 F4 90.65(14) . . ?
F6 P3 F3 89.65(14) . . ?
F5 P3 F3 90.88(13) . . ?
F4 P3 F3 178.35(13) . . ?
F6 P3 F1 178.74(15) . . ?
F5 P3 F1 90.17(14) . . ?
F4 P3 F1 89.09(15) . . ?
F3 P3 F1 90.28(15) . . ?
F6 P3 F2 90.78(14) . . ?
F5 P3 F2 178.13(14) . . ?
F4 P3 F2 89.51(13) . . ?
F3 P3 F2 88.94(13) . . ?
F1 P3 F2 87.97(14) . . ?
C5 N1 Co1 127.7(2) . . ?
C5 N1 H1A 105.4 . . ?
Co1 N1 H1A 105.4 . . ?
C5 N1 H1B 105.4 . . ?
Co1 N1 H1B 105.4 . . ?
H1A N1 H1B 106.0 . . ?
C10 N2 Co1 124.76(19) . . ?
C10 N2 H2A 106.1 . . ?
Co1 N2 H2A 106.1 . . ?
C10 N2 H2B 106.1 . . ?
Co1 N2 H2B 106.1 . . ?
H2A N2 H2B 106.3 . . ?
P1 C1 H1C 109.5 . . ?
P1 C1 H1D 109.5 . . ?
H1C C1 H1D 109.5 . . ?
P1 C1 H1E 109.5 . . ?
H1C C1 H1E 109.5 . . ?
H1D C1 H1E 109.5 . . ?
P1 C2 H2C 109.5 . . ?
P1 C2 H2D 109.5 . . ?
H2C C2 H2D 109.5 . . ?
P1 C2 H2E 109.5 . . ?
H2C C2 H2E 109.5 . . ?
H2D C2 H2E 109.5 . . ?
C4 C3 P1 115.5(2) . . ?
C4 C3 H3A 108.4 . . ?
P1 C3 H3A 108.4 . . ?
C4 C3 H3B 108.4 . . ?
P1 C3 H3B 108.4 . . ?
H3A C3 H3B 107.5 . . ?
C5 C4 C3 112.8(3) . . ?
C5 C4 H4A 109.0 . . ?
C3 C4 H4A 109.0 . . ?
C5 C4 H4B 109.0 . . ?
C3 C4 H4B 109.0 . . ?
H4A C4 H4B 107.8 . . ?
N1 C5 C4 112.3(3) . . ?
N1 C5 H5A 109.1 . . ?
C4 C5 H5A 109.1 . . ?
N1 C5 H5B 109.1 . . ?
C4 C5 H5B 109.1 . . ?
H5A C5 H5B 107.9 . . ?
P2 C6 H6A 109.5 . . ?
P2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
P2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
P2 C7 H7A 109.5 . . ?
P2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
P2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 P2 116.5(2) . . ?
C9 C8 H8A 108.2 . . ?
P2 C8 H8A 108.2 . . ?
C9 C8 H8B 108.2 . . ?
P2 C8 H8B 108.2 . . ?
H8A C8 H8B 107.3 . . ?
C10 C9 C8 113.1(3) . . ?
C10 C9 H9A 109.0 . . ?
C8 C9 H9A 109.0 . . ?
C10 C9 H9B 109.0 . . ?
C8 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
N2 C10 C9 111.3(3) . . ?
N2 C10 H10A 109.4 . . ?
C9 C10 H10A 109.4 . . ?
N2 C10 H10B 109.4 . . ?
C9 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
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 N2 2.049(3) . ?
Co1 N1 2.053(3) . ?
Co1 P2 2.223(2) . ?
Co1 P1 2.225(2) . ?
Co1 Cl2 2.246(2) . ?
Co1 Cl1 2.252(2) . ?
P1 C1 1.802(3) . ?
P1 C2 1.808(3) . ?
P1 C3 1.819(3) . ?
P2 C7 1.815(4) . ?
P2 C6 1.818(4) . ?
P2 C8 1.826(4) . ?
P3 F6 1.573(3) . ?
P3 F5 1.579(3) . ?
P3 F4 1.594(3) . ?
P3 F3 1.597(3) . ?
P3 F1 1.598(3) . ?
P3 F2 1.604(3) . ?
N1 C5 1.476(4) . ?
N1 H1A 0.9200 . ?
N1 H1B 0.9200 . ?
N2 C10 1.481(4) . ?
N2 H2A 0.9200 . ?
N2 H2B 0.9200 . ?
C1 H1C 0.9800 . ?
C1 H1D 0.9800 . ?
C1 H1E 0.9800 . ?
C2 H2C 0.9800 . ?
C2 H2D 0.9800 . ?
C2 H2E 0.9800 . ?
C3 C4 1.515(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.508(5) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.529(5) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.503(5) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Co1 P1 C1 -147.36(14) . . . . ?
P2 Co1 P1 C1 40.07(13) . . . . ?
Cl2 Co1 P1 C1 -55.31(15) . . . . ?
Cl1 Co1 P1 C1 126.91(14) . . . . ?
N1 Co1 P1 C2 87.51(17) . . . . ?
P2 Co1 P1 C2 -85.06(15) . . . . ?
Cl2 Co1 P1 C2 179.56(13) . . . . ?
Cl1 Co1 P1 C2 1.78(13) . . . . ?
N1 Co1 P1 C3 -31.70(14) . . . . ?
P2 Co1 P1 C3 155.72(12) . . . . ?
Cl2 Co1 P1 C3 60.34(12) . . . . ?
Cl1 Co1 P1 C3 -117.43(12) . . . . ?
N2 Co1 P2 C7 82.69(19) . . . . ?
P1 Co1 P2 C7 -89.64(17) . . . . ?
Cl2 Co1 P2 C7 -3.44(15) . . . . ?
Cl1 Co1 P2 C7 176.85(15) . . . . ?
N2 Co1 P2 C6 -150.69(15) . . . . ?
P1 Co1 P2 C6 36.98(13) . . . . ?
Cl2 Co1 P2 C6 123.18(15) . . . . ?
Cl1 Co1 P2 C6 -56.53(15) . . . . ?
N2 Co1 P2 C8 -35.45(14) . . . . ?
P1 Co1 P2 C8 152.22(12) . . . . ?
Cl2 Co1 P2 C8 -121.59(13) . . . . ?
Cl1 Co1 P2 C8 58.71(13) . . . . ?
N2 Co1 N1 C5 -129.0(3) . . . . ?
P1 Co1 N1 C5 42.9(3) . . . . ?
Cl2 Co1 N1 C5 -42.8(3) . . . . ?
Cl1 Co1 N1 C5 136.8(3) . . . . ?
N1 Co1 N2 C10 -120.1(2) . . . . ?
P2 Co1 N2 C10 51.9(2) . . . . ?
Cl2 Co1 N2 C10 147.7(2) . . . . ?
Cl1 Co1 N2 C10 -34.5(2) . . . . ?
C1 P1 C3 C4 176.9(2) . . . . ?
C2 P1 C3 C4 -75.2(3) . . . . ?
Co1 P1 C3 C4 51.6(3) . . . . ?
P1 C3 C4 C5 -67.0(3) . . . . ?
Co1 N1 C5 C4 -62.8(4) . . . . ?
C3 C4 C5 N1 68.0(4) . . . . ?
C7 P2 C8 C9 -75.1(3) . . . . ?
C6 P2 C8 C9 176.1(2) . . . . ?
Co1 P2 C8 C9 49.9(3) . . . . ?
P2 C8 C9 C10 -62.1(3) . . . . ?
Co1 N2 C10 C9 -71.5(3) . . . . ?
C8 C9 C10 N2 67.9(3) . . . . ?
