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#$Date: 2016-03-25 09:31:10 +0100 (vie 25 de mar de 2016) $
#$Revision: 179752 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/48/7004853.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_7004853
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-, C2 H3 N'
_chemical_formula_sum            'C12 H31 Cl2 Co F6 N3 P3'
_chemical_formula_weight         554.14
_chemical_name_common
;
trans(Cl,Cl)cis(P,P)-dichlorobis((3-
aminopropyl)dimethylphosphine)cobalt(iii) hexafluorophosphate
acetonitrile solvate
;
_chemical_name_systematic
;
trans(Cl,Cl)cis(P,P)-dichlorobis((3-aminopropyl)dimethylphosphine)cobalt(III)
hexafluorophosphate acetonitrile solvate
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_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                 104.58(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.771(9)
_cell_length_b                   17.947(8)
_cell_length_c                   7.952(4)
_cell_measurement_reflns_used    8517
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.2
_cell_volume                     2316(2)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_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      296(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0199
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            11386
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         3.16
_exptl_absorpt_coefficient_mu    1.230
_exptl_absorpt_correction_T_max  0.7910
_exptl_absorpt_correction_T_min  0.7485
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Higashi, T. (1995). Program for Absorption Correction.
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.890
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         2738
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0543
_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)+(0.0667P)²+11.8368P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1660
_refine_ls_wR_factor_ref         0.1745
_reflns_number_gt                2362
_reflns_number_total             2738
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            b612025c.txt
_cod_data_source_block           pdmpCl2C
_cod_database_code               7004853
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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 1.0000 0.22206(4) 1.0000 0.0340(2) Uani 1 2 d S . .
Cl1 Cl 1.09068(7) 0.21842(8) 0.83557(15) 0.0559(3) Uani 1 1 d . . .
P1 P 0.93058(7) 0.30759(7) 0.81650(15) 0.0467(3) Uani 1 1 d . . .
P2 P 0.70303(12) 0.0000 0.7034(3) 0.0551(5) Uani 1 2 d S . .
F1 F 0.7029(5) -0.0862(3) 0.7087(13) 0.193(4) Uani 1 1 d . . .
F2 F 0.6109(4) 0.0000 0.5968(9) 0.147(3) Uani 1 2 d S . .
F3 F 0.6692(4) 0.0000 0.8726(7) 0.0925(17) Uani 1 2 d S . .
F4 F 0.7343(5) 0.0000 0.5355(9) 0.160(4) Uani 1 2 d S . .
F5 F 0.7949(4) 0.0000 0.8051(10) 0.132(3) Uani 1 2 d S . .
N1 N 0.9308(3) 0.1387(2) 0.8520(5) 0.0522(9) Uani 1 1 d . . .
H1A H 0.9576 0.0959 0.8887 0.063 Uiso 1 1 calc R . .
H1B H 0.8834 0.1368 0.8855 0.063 Uiso 1 1 calc R . .
N2 N 0.9587(9) 0.0000 1.1623(18) 0.123(4) Uani 1 2 d S . .
C1 C 0.8386(4) 0.3447(4) 0.8613(8) 0.0793(19) Uani 1 1 d . . .
H1C H 0.8056 0.3046 0.8868 0.095 Uiso 1 1 calc R . .
H1D H 0.8078 0.3716 0.7617 0.095 Uiso 1 1 calc R . .
H1E H 0.8532 0.3776 0.9593 0.095 Uiso 1 1 calc R . .
C2 C 0.9866(5) 0.3891(3) 0.7682(9) 0.084(2) Uani 1 1 d . . .
H2A H 1.0369 0.3733 0.7424 0.101 Uiso 1 1 calc R . .
H2B H 0.9991 0.4217 0.8670 0.101 Uiso 1 1 calc R . .
H2C H 0.9532 0.4150 0.6698 0.101 Uiso 1 1 calc R . .
C3 C 0.8928(3) 0.2714(3) 0.5988(6) 0.0543(12) Uani 1 1 d . . .
H3A H 0.8553 0.3078 0.5311 0.065 Uiso 1 1 calc R . .
H3B H 0.9391 0.2669 0.5470 0.065 Uiso 1 1 calc R . .
C4 C 0.8488(3) 0.1968(3) 0.5818(6) 0.0612(13) Uani 1 1 d . . .
H4A H 0.8251 0.1861 0.4598 0.073 Uiso 1 1 calc R . .
H4B H 0.8041 0.1995 0.6388 0.073 Uiso 1 1 calc R . .
C5 C 0.9067(3) 0.1338(3) 0.6618(6) 0.0577(12) Uani 1 1 d . . .
H5A H 0.8798 0.0864 0.6274 0.069 Uiso 1 1 calc R . .
H5B H 0.9557 0.1359 0.6180 0.069 Uiso 1 1 calc R . .
C6 C 0.9034(7) 0.0000 1.201(2) 0.100(4) Uani 1 2 d S . .
C7 C 0.8274(11) 0.0000 1.231(2) 0.156(7) Uani 1 2 d S . .
H7A H 0.8002 0.0461 1.1913 0.188 Uiso 0.50 1 calc PR . .
H7B H 0.8323 -0.0054 1.3534 0.188 Uiso 0.50 1 calc PR . .
H7C H 0.7959 -0.0407 1.1698 0.188 Uiso 0.50 1 calc PR . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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
N1 Co1 N1 87.4(2) . 2_757 ?
N1 Co1 P1 89.99(13) . . ?
N1 Co1 P1 173.81(11) 2_757 . ?
N1 Co1 P1 173.81(11) . 2_757 ?
N1 Co1 P1 89.98(13) 2_757 2_757 ?
P1 Co1 P1 93.14(7) . 2_757 ?
N1 Co1 Cl1 86.85(13) . 2_757 ?
N1 Co1 Cl1 90.75(13) 2_757 2_757 ?
P1 Co1 Cl1 94.73(6) . 2_757 ?
P1 Co1 Cl1 87.57(6) 2_757 2_757 ?
N1 Co1 Cl1 90.74(13) . . ?
N1 Co1 Cl1 86.84(13) 2_757 . ?
P1 Co1 Cl1 87.57(6) . . ?
P1 Co1 Cl1 94.73(6) 2_757 . ?
Cl1 Co1 Cl1 176.67(8) 2_757 . ?
C1 P1 C3 102.2(3) . . ?
C1 P1 C2 104.9(4) . . ?
C3 P1 C2 99.2(3) . . ?
C1 P1 Co1 117.2(2) . . ?
C3 P1 Co1 112.24(18) . . ?
C2 P1 Co1 118.4(2) . . ?
F1 P2 F1 176.9(7) . 6 ?
F1 P2 F5 89.6(4) . . ?
F1 P2 F5 89.6(4) 6 . ?
F1 P2 F4 91.5(3) . . ?
F1 P2 F4 91.5(3) 6 . ?
F5 P2 F4 86.7(5) . . ?
F1 P2 F2 90.4(4) . . ?
F1 P2 F2 90.4(4) 6 . ?
F5 P2 F2 178.7(4) . . ?
F4 P2 F2 92.0(4) . . ?
F1 P2 F3 88.5(3) . . ?
F1 P2 F3 88.5(3) 6 . ?
F5 P2 F3 94.5(4) . . ?
F4 P2 F3 178.8(4) . . ?
F2 P2 F3 86.8(4) . . ?
C5 N1 Co1 126.8(3) . . ?
C5 N1 H1A 105.6 . . ?
Co1 N1 H1A 105.6 . . ?
C5 N1 H1B 105.6 . . ?
Co1 N1 H1B 105.6 . . ?
H1A N1 H1B 106.1 . . ?
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 H2A 109.5 . . ?
P1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
P1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 P1 116.5(3) . . ?
C4 C3 H3A 108.2 . . ?
P1 C3 H3A 108.2 . . ?
C4 C3 H3B 108.2 . . ?
P1 C3 H3B 108.2 . . ?
H3A C3 H3B 107.3 . . ?
C3 C4 C5 111.9(4) . . ?
C3 C4 H4A 109.2 . . ?
C5 C4 H4A 109.2 . . ?
C3 C4 H4B 109.2 . . ?
C5 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
N1 C5 C4 111.6(4) . . ?
N1 C5 H5A 109.3 . . ?
C4 C5 H5A 109.3 . . ?
N1 C5 H5B 109.3 . . ?
C4 C5 H5B 109.3 . . ?
H5A C5 H5B 108.0 . . ?
N2 C6 C7 173(2) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
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 N1 2.070(4) . ?
Co1 N1 2.070(4) 2_757 ?
Co1 P1 2.2328(14) . ?
Co1 P1 2.2328(14) 2_757 ?
Co1 Cl1 2.2422(14) 2_757 ?
Co1 Cl1 2.2423(14) . ?
P1 C1 1.796(6) . ?
P1 C3 1.808(5) . ?
P1 C2 1.831(6) . ?
P2 F1 1.548(5) . ?
P2 F1 1.548(5) 6 ?
P2 F5 1.550(6) . ?
P2 F4 1.553(6) . ?
P2 F2 1.564(7) . ?
P2 F3 1.586(6) . ?
N1 C5 1.466(6) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N2 C6 1.050(14) . ?
C1 H1C 0.9600 . ?
C1 H1D 0.9600 . ?
C1 H1E 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 C4 1.519(7) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.521(8) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C7 1.353(18) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
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 89.6(3) . . . . ?
P1 Co1 P1 C1 -85.0(3) 2_757 . . . ?
Cl1 Co1 P1 C1 2.8(3) 2_757 . . . ?
Cl1 Co1 P1 C1 -179.6(3) . . . . ?
N1 Co1 P1 C3 -28.3(2) . . . . ?
P1 Co1 P1 C3 157.1(2) 2_757 . . . ?
Cl1 Co1 P1 C3 -115.1(2) 2_757 . . . ?
Cl1 Co1 P1 C3 62.49(19) . . . . ?
N1 Co1 P1 C2 -143.0(3) . . . . ?
P1 Co1 P1 C2 42.4(3) 2_757 . . . ?
Cl1 Co1 P1 C2 130.2(3) 2_757 . . . ?
Cl1 Co1 P1 C2 -52.2(3) . . . . ?
N1 Co1 N1 C5 -132.4(5) 2_757 . . . ?
P1 Co1 N1 C5 41.9(4) . . . . ?
Cl1 Co1 N1 C5 136.7(4) 2_757 . . . ?
Cl1 Co1 N1 C5 -45.6(4) . . . . ?
C1 P1 C3 C4 -78.6(5) . . . . ?
C2 P1 C3 C4 173.8(4) . . . . ?
Co1 P1 C3 C4 47.8(5) . . . . ?
P1 C3 C4 C5 -66.3(5) . . . . ?
Co1 N1 C5 C4 -65.3(6) . . . . ?
C3 C4 C5 N1 70.9(6) . . . . ?
