#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/80/2238021.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_2238021
loop_
_publ_author_name
'Reiss, Guido J.'
_publ_section_title
;
 trans-Dichloridotetrakis[(dimethylphosphoryl)methanaminium-κO]cobalt(II)
 tetrachloridocobaltate(II)
;
_journal_coeditor_code           SJ5313
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m248
_journal_page_last               m249
_journal_paper_doi               10.1107/S1600536813008945
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Co Cl2 (C3 H11 N O P)4] [Co Cl4]2'
_chemical_formula_moiety         'C12 H44 Cl2 Co1 N4 O4 P4 4+, 2(Cl4 Co 2-)'
_chemical_formula_sum            'C12 H44 Cl10 Co3 N4 O4 P4'
_chemical_formula_weight         963.68
_chemical_name_systematic
'trans-Dichloridotetrakis[(dimethylphosphoryl)methanaminium-κO]cobalt(II) bis[tetrachloridocobaltate(II)]'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                110.738(4)
_cell_angle_beta                 97.688(4)
_cell_angle_gamma                104.331(5)
_cell_formula_units_Z            1
_cell_length_a                   7.7748(3)
_cell_length_b                   11.1557(5)
_cell_length_c                   12.1205(5)
_cell_measurement_reflns_used    13303
_cell_measurement_temperature    173.0(10)
_cell_measurement_theta_max      32.6097
_cell_measurement_theta_min      2.8862
_cell_volume                     923.67(8)
_computing_cell_refinement       'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2012)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.0(10)
_diffrn_detector_area_resol_mean 16.2711
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Oxford Xcalibur'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0202
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15687
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.997
_diffrn_reflns_theta_min         2.892
_exptl_absorpt_coefficient_mu    2.254
_exptl_absorpt_correction_T_max  0.838
_exptl_absorpt_correction_T_min  0.402
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[CrysAlis PRO (Oxford Diffraction, 2009), based on expressions derived
by Clark & Reid (1995)]
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.732
_exptl_crystal_description       block
_exptl_crystal_F_000             487
_exptl_crystal_size_max          0.759
_exptl_crystal_size_mid          0.331
_exptl_crystal_size_min          0.079
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.381
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         4920
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0211
_refine_ls_R_factor_gt           0.0183
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[σ²(Fo²)+(0.012P)²+0.50P], where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0405
_refine_ls_wR_factor_ref         0.0416
_reflns_number_gt                4552
_reflns_number_total             4920
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            sj5313.cif
_cod_data_source_block           I
_cod_original_cell_volume        923.66(8)
_cod_database_code               2238021
_cod_database_fobs_code          2238021
#BEGIN Tags that were not found in dictionaries:
_shelxl_version_number           20.13
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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_occupancy
Co Co1 0.0000 0.0000 0.5000 0.00707(5) Uani d 1
Cl Cl1 -0.22848(4) 0.05961(3) 0.61151(3) 0.01037(6) Uani d 1
P P1 0.27356(4) -0.01270(3) 0.73117(3) 0.00824(6) Uani d 1
C C11 0.48106(18) 0.09673(14) 0.84045(13) 0.0149(3) Uani d 1
H H11A 0.5714 0.1238 0.7997 0.022 Uiso calc 1
H H11B 0.5241 0.0503 0.8858 0.022 Uiso calc 1
H H11C 0.4599 0.1753 0.8949 0.022 Uiso calc 1
C C12 0.31916(19) -0.15805(14) 0.63526(13) 0.0149(3) Uani d 1
H H12A 0.2069 -0.2229 0.5800 0.022 Uiso calc 1
H H12B 0.3725 -0.1973 0.6841 0.022 Uiso calc 1
H H12C 0.4027 -0.1323 0.5899 0.022 Uiso calc 1
C C13 0.11865(17) -0.06627(14) 0.81714(12) 0.0117(2) Uani d 1
H H13A 0.1385 -0.1437 0.8293 0.014 Uiso calc 1
H H13B 0.1417 0.0064 0.8963 0.014 Uiso calc 1
N N1 -0.07340(15) -0.10285(12) 0.74832(11) 0.0112(2) Uani d 1
H H11 -0.093(2) -0.0313(19) 0.7437(17) 0.022(5) Uiso d 1
H H12 -0.094(3) -0.162(2) 0.6731(19) 0.026(5) Uiso d 1
H H13 -0.149(3) -0.1352(19) 0.7854(18) 0.024(5) Uiso d 1
O O1 0.18513(12) 0.05528(9) 0.66322(8) 0.00960(17) Uani d 1
P P2 0.25797(4) 0.32277(3) 0.61086(3) 0.00895(6) Uani d 1
C C21 0.2810(2) 0.47433(13) 0.58704(13) 0.0158(3) Uani d 1
H H21A 0.3016 0.4603 0.5077 0.024 Uiso calc 1
H H21B 0.3827 0.5461 0.6477 0.024 Uiso calc 1
H H21C 0.1710 0.4981 0.5929 0.024 Uiso calc 1
C C22 0.47331(18) 0.29394(14) 0.61459(13) 0.0152(3) Uani d 1
H H22A 0.4593 0.2039 0.6092 0.023 Uiso calc 1
H H22B 0.5591 0.3581 0.6894 0.023 Uiso calc 1
H H22C 0.5177 0.3043 0.5472 0.023 Uiso calc 1
C C23 0.22948(18) 0.36089(13) 0.76527(12) 0.0119(2) Uani d 1
H H23A 0.2637 0.2967 0.7933 0.014 Uiso calc 1
H H23B 0.3122 0.4504 0.8183 0.014 Uiso calc 1
N N2 0.03979(16) 0.35581(12) 0.77545(11) 0.0122(2) Uani d 1
H H21 0.003(2) 0.4202(18) 0.7562(17) 0.019(4) Uiso d 1
H H22 -0.041(2) 0.2708(19) 0.7275(17) 0.018(4) Uiso d 1
H H23 0.035(3) 0.3711(19) 0.8492(19) 0.026(5) Uiso d 1
O O2 0.10036(12) 0.20618(9) 0.51575(8) 0.00961(17) Uani d 1
Co Co2 0.17901(2) 0.34799(2) 0.10713(2) 0.01000(4) Uani d 1
Cl Cl21 0.08194(5) 0.41433(3) 0.28405(3) 0.01496(7) Uani d 1
Cl Cl22 0.27225(5) 0.53299(3) 0.06796(3) 0.01464(7) Uani d 1
Cl Cl23 0.38534(4) 0.24331(3) 0.14315(3) 0.01438(7) Uani d 1
Cl Cl24 -0.04975(4) 0.19017(3) -0.05026(3) 0.01361(6) Uani d 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'
O O 0.0106 0.0060 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O1 Co1 O1 2_556 . 180.00(4)
O1 Co1 O2 2_556 2_556 88.92(3)
O1 Co1 O2 . 2_556 91.08(3)
O1 Co1 O2 2_556 . 91.08(3)
O1 Co1 O2 . . 88.92(3)
O2 Co1 O2 2_556 . 180.0
O1 Co1 Cl1 2_556 2_556 89.89(3)
O1 Co1 Cl1 . 2_556 90.11(3)
O2 Co1 Cl1 2_556 2_556 89.54(3)
O2 Co1 Cl1 . 2_556 90.46(3)
O1 Co1 Cl1 2_556 . 90.11(3)
O1 Co1 Cl1 . . 89.88(3)
O2 Co1 Cl1 2_556 . 90.46(3)
O2 Co1 Cl1 . . 89.54(3)
Cl1 Co1 Cl1 2_556 . 180.0
O1 P1 C11 . . 113.52(6)
O1 P1 C12 . . 113.89(6)
C11 P1 C12 . . 107.60(7)
O1 P1 C13 . . 108.03(6)
C11 P1 C13 . . 105.63(6)
C12 P1 C13 . . 107.70(7)
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
N1 C13 P1 . . 108.91(9)
N1 C13 H13A . . 109.9
P1 C13 H13A . . 109.9
N1 C13 H13B . . 109.9
P1 C13 H13B . . 109.9
H13A C13 H13B . . 108.3
C13 N1 H11 . . 109.2(12)
C13 N1 H12 . . 111.8(12)
H11 N1 H12 . . 106.4(17)
C13 N1 H13 . . 109.9(13)
H11 N1 H13 . . 109.5(17)
H12 N1 H13 . . 109.9(17)
P1 O1 Co1 . . 138.08(6)
O2 P2 C22 . . 113.83(6)
O2 P2 C21 . . 111.21(6)
C22 P2 C21 . . 107.23(7)
O2 P2 C23 . . 112.87(6)
C22 P2 C23 . . 104.79(6)
C21 P2 C23 . . 106.37(6)
P2 C21 H21A . . 109.5
P2 C21 H21B . . 109.5
H21A C21 H21B . . 109.5
P2 C21 H21C . . 109.5
H21A C21 H21C . . 109.5
H21B C21 H21C . . 109.5
P2 C22 H22A . . 109.5
P2 C22 H22B . . 109.5
H22A C22 H22B . . 109.5
P2 C22 H22C . . 109.5
H22A C22 H22C . . 109.5
H22B C22 H22C . . 109.5
N2 C23 P2 . . 113.44(9)
N2 C23 H23A . . 108.9
P2 C23 H23A . . 108.9
N2 C23 H23B . . 108.9
P2 C23 H23B . . 108.9
H23A C23 H23B . . 107.7
C23 N2 H21 . . 112.8(11)
C23 N2 H22 . . 110.3(11)
H21 N2 H22 . . 110.3(16)
C23 N2 H23 . . 108.5(13)
H21 N2 H23 . . 107.4(17)
H22 N2 H23 . . 107.3(17)
P2 O2 Co1 . . 128.45(5)
Cl22 Co2 Cl24 . . 108.699(15)
Cl22 Co2 Cl23 . . 119.352(15)
Cl24 Co2 Cl23 . . 106.345(14)
Cl22 Co2 Cl21 . . 106.654(14)
Cl24 Co2 Cl21 . . 111.513(15)
Cl23 Co2 Cl21 . . 104.233(14)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Co1 O1 2_556 2.0737(9)
Co1 O1 . 2.0737(9)
Co1 O2 2_556 2.1671(9)
Co1 O2 . 2.1671(9)
Co1 Cl1 2_556 2.4525(3)
Co1 Cl1 . 2.4526(3)
P1 O1 . 1.5083(9)
P1 C11 . 1.7763(14)
P1 C12 . 1.7794(14)
P1 C13 . 1.8204(13)
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 N1 . 1.4886(17)
C13 H13A . 0.9700
C13 H13B . 0.9700
N1 H11 . 0.867(19)
N1 H12 . 0.88(2)
N1 H13 . 0.87(2)
P2 O2 . 1.5144(9)
P2 C22 . 1.7791(14)
P2 C21 . 1.7843(14)
P2 C23 . 1.8238(14)
C21 H21A . 0.9600
C21 H21B . 0.9600
C21 H21C . 0.9600
C22 H22A . 0.9600
C22 H22B . 0.9600
C22 H22C . 0.9600
C23 N2 . 1.4852(17)
C23 H23A . 0.9700
C23 H23B . 0.9700
N2 H21 . 0.924(19)
N2 H22 . 0.920(19)
N2 H23 . 0.86(2)
Co2 Cl22 . 2.2485(4)
Co2 Cl24 . 2.2507(4)
Co2 Cl23 . 2.2866(4)
Co2 Cl21 . 2.3024(4)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H11 Cl1 . 0.867(19) 2.437(19) 3.1879(12) 145.3(16)
N1 H11 Cl24 1_556 0.867(19) 2.730(19) 3.2573(13) 120.5(15)
N1 H12 O2 2_556 0.88(2) 2.16(2) 2.9504(16) 150.3(17)
N1 H13 Cl23 2_556 0.87(2) 2.38(2) 3.2403(12) 171.3(17)
N2 H22 Cl1 . 0.920(19) 2.250(19) 3.1697(13) 177.8(15)
N2 H21 Cl21 2_566 0.924(19) 2.288(19) 3.2124(12) 177.8(16)
N2 H23 Cl22 1_556 0.86(2) 2.71(2) 3.3612(13) 134.0(16)
N2 H23 Cl24 1_556 0.86(2) 2.70(2) 3.2989(12) 128.1(16)
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
O1 P1 C13 N1 32.47(10)
C11 P1 C13 N1 154.27(9)
C12 P1 C13 N1 -90.96(10)
C11 P1 O1 Co1 158.09(8)
C12 P1 O1 Co1 34.48(10)
C13 P1 O1 Co1 -85.12(9)
O2 P2 C23 N2 -41.65(11)
C22 P2 C23 N2 -166.05(9)
C21 P2 C23 N2 80.57(10)
C22 P2 O2 Co1 60.81(9)
C21 P2 O2 Co1 -177.94(7)
C23 P2 O2 Co1 -58.48(8)
