#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/97/2229783.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_2229783
loop_
_publ_author_name
'Xu, Xiaofeng'
'Feng, Lei'
'Li, Xiaoyan'
_publ_section_title
;
 Cyanidotetrakis(trimethylphosphine)cobalt(I)
;
_journal_coeditor_code           OM2401
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m503
_journal_paper_doi               10.1107/S160053681101083X
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Co (CN) (C3 H9 P)4]'
_chemical_formula_moiety         'C13 H36 Co N P4'
_chemical_formula_sum            'C13 H36 Co N P4'
_chemical_formula_weight         389.24
_chemical_name_systematic
;
Cyanidotetrakis(trimethylphosphine)cobalt(I)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 93.09(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.160(3)
_cell_length_b                   9.6136(19)
_cell_length_c                   17.971(4)
_cell_measurement_reflns_used    4976
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.27
_cell_volume                     2270.3(9)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2001)'
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEXII'
_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  0.0197
_diffrn_reflns_av_sigmaI/netI    0.0239
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11732
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    1.029
_exptl_absorpt_correction_T_max  0.4335
_exptl_absorpt_correction_T_min  0.3951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.139
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             832.0
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.060
_refine_diff_density_min         -2.002
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         4438
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.168
_refine_ls_R_factor_all          0.0786
_refine_ls_R_factor_gt           0.0681
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1278P)²+4.3800P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2018
_refine_ls_wR_factor_ref         0.2155
_reflns_number_gt                3663
_reflns_number_total             4438
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2401.cif
_cod_data_source_block           I
_cod_original_cell_volume        2270.3(8)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2229783
_cod_database_fobs_code          2229783
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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 0.0427(7) 0.5719(11) 0.6108(6) 0.112(3) Uani d U 1 A .
H H1A -0.0142 0.5545 0.6407 0.167 Uiso calc R 1 . .
H H1B 0.0756 0.4855 0.6002 0.167 Uiso calc R 1 . .
H H1C 0.0194 0.6154 0.5649 0.167 Uiso calc R 1 . .
C C2 0.1727(9) 0.5681(11) 0.7382(6) 0.125(4) Uani d U 1 A .
H H2A 0.2114 0.6174 0.7766 0.187 Uiso calc R 1 . .
H H2B 0.2134 0.4948 0.7192 0.187 Uiso calc R 1 . .
H H2C 0.1130 0.5292 0.7585 0.187 Uiso calc R 1 . .
C C3 0.0419(8) 0.7949(12) 0.7113(7) 0.123(4) Uani d U 1 A 1
H H3A -0.0118 0.7361 0.7271 0.184 Uiso calc R 1 A 1
H H3B 0.0140 0.8651 0.6782 0.184 Uiso calc R 1 A 1
H H3C 0.0754 0.8383 0.7540 0.184 Uiso calc R 1 A 1
C C4 0.3468(6) 0.7624(9) 0.4375(4) 0.080(2) Uani d U 1 A .
H H4A 0.4136 0.7418 0.4588 0.120 Uiso calc R 1 . .
H H4B 0.3416 0.8603 0.4273 0.120 Uiso calc R 1 . .
H H4C 0.3353 0.7112 0.3920 0.120 Uiso calc R 1 . .
C C5 0.1325(6) 0.7398(9) 0.4449(4) 0.0768(19) Uani d U 1 A .
H H5A 0.1354 0.6858 0.4002 0.115 Uiso calc R 1 . .
H H5B 0.1263 0.8366 0.4323 0.115 Uiso calc R 1 . .
H H5C 0.0748 0.7115 0.4716 0.115 Uiso calc R 1 . .
C C6 0.2570(7) 0.5211(8) 0.4942(4) 0.080(2) Uani d U 1 A .
H H6A 0.1998 0.4794 0.5167 0.120 Uiso calc R 1 . .
H H6B 0.3189 0.4877 0.5186 0.120 Uiso calc R 1 . .
H H6C 0.2557 0.4971 0.4424 0.120 Uiso calc R 1 . .
C C7 0.5231(5) 0.8559(9) 0.6188(4) 0.0783(9) Uani d U 1 A 1
H H7A 0.5086 0.8925 0.5697 0.117 Uiso calc R 1 A 1
H H7B 0.5871 0.8078 0.6203 0.117 Uiso calc R 1 A 1
H H7C 0.5264 0.9309 0.6541 0.117 Uiso calc R 1 A 1
C C8 0.4623(6) 0.7086(8) 0.7401(4) 0.0771(9) Uani d U 1 A 1
H H8A 0.4308 0.6273 0.7597 0.116 Uiso calc R 1 A 1
H H8B 0.4438 0.7887 0.7682 0.116 Uiso calc R 1 A 1
H H8C 0.5349 0.6975 0.7436 0.116 Uiso calc R 1 A 1
C C9 0.4766(5) 0.5759(8) 0.6060(4) 0.0770(9) Uani d U 1 A 1
H H9A 0.5466 0.5704 0.6237 0.115 Uiso calc R 1 A 1
H H9B 0.4727 0.5797 0.5525 0.115 Uiso calc R 1 A 1
H H9C 0.4407 0.4954 0.6222 0.115 Uiso calc R 1 A 1
C C10 0.1996(9) 1.0851(10) 0.4832(5) 0.114(3) Uani d U 1 A 1
H H10A 0.1993 1.1849 0.4826 0.172 Uiso calc R 1 A 1
H H10B 0.1330 1.0512 0.4683 0.172 Uiso calc R 1 A 1
H H10C 0.2479 1.0513 0.4493 0.172 Uiso calc R 1 A 1
C C11 0.1338(10) 1.1173(12) 0.6267(7) 0.134(3) Uani d U 1 A 1
H H11A 0.1330 1.0866 0.6775 0.201 Uiso calc R 1 A 1
H H11B 0.0691 1.0984 0.6016 0.201 Uiso calc R 1 A 1
H H11C 0.1470 1.2154 0.6255 0.201 Uiso calc R 1 A 1
C C12 0.3430(9) 1.1417(11) 0.5971(7) 0.123(3) Uani d U 1 A 1
H H12A 0.4025 1.1046 0.5757 0.185 Uiso calc R 1 A 1
H H12B 0.3557 1.1521 0.6499 0.185 Uiso calc R 1 A 1
H H12C 0.3270 1.2308 0.5754 0.185 Uiso calc R 1 A 1
C C13 0.2731(5) 0.8878(6) 0.7120(3) 0.0545(13) Uani d U 1 . .
Co Co1 0.26139(5) 0.80567(6) 0.61596(3) 0.0371(3) Uani d . 1 A .
N N1 0.2797(6) 0.9405(7) 0.7705(3) 0.0869(19) Uani d . 1 . .
P P1 0.13485(13) 0.68895(18) 0.66233(9) 0.0621(5) Uani d . 1 . .
P P2 0.25026(12) 0.71209(15) 0.50400(7) 0.0479(4) Uani d . 1 . .
P P3 0.41947(12) 0.7316(2) 0.64284(9) 0.0605(4) Uani d U 1 . .
P P4 0.23568(14) 1.02279(15) 0.57888(9) 0.0598(4) Uani d U 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'
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'
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
P1 C1 H1A . . 109.5 ?
P1 C1 H1B . . 109.5 ?
H1A C1 H1B . . 109.5 ?
P1 C1 H1C . . 109.5 ?
H1A C1 H1C . . 109.5 ?
H1B C1 H1C . . 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 ?
P1 C3 H3A . . 109.5 ?
P1 C3 H3B . . 109.5 ?
P1 C3 H3C . . 109.5 ?
P2 C4 H4A . . 109.5 ?
P2 C4 H4B . . 109.5 ?
H4A C4 H4B . . 109.5 ?
P2 C4 H4C . . 109.5 ?
H4A C4 H4C . . 109.5 ?
H4B C4 H4C . . 109.5 ?
P2 C5 H5A . . 109.5 ?
P2 C5 H5B . . 109.5 ?
H5A C5 H5B . . 109.5 ?
P2 C5 H5C . . 109.5 ?
H5A C5 H5C . . 109.5 ?
H5B C5 H5C . . 109.5 ?
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 ?
P3 C7 H7A . . 109.5 ?
P3 C7 H7B . . 109.5 ?
P3 C7 H7C . . 109.5 ?
P3 C8 H8A . . 109.5 ?
P3 C8 H8B . . 109.5 ?
P3 C8 H8C . . 109.5 ?
P3 C9 H9A . . 109.5 ?
P3 C9 H9B . . 109.5 ?
P3 C9 H9C . . 109.5 ?
P4 C10 H10A . . 109.5 ?
P4 C10 H10B . . 109.5 ?
P4 C10 H10C . . 109.5 ?
P4 C11 H11A . . 109.5 ?
P4 C11 H11B . . 109.5 ?
P4 C11 H11C . . 109.5 ?
P4 C12 H12A . . 109.5 ?
P4 C12 H12B . . 109.5 ?
P4 C12 H12C . . 109.5 ?
N1 C13 Co1 . . 178.8(6) y
C13 Co1 P2 . . 179.02(19) y
C13 Co1 P1 . . 83.92(19) y
P2 Co1 P1 . . 97.05(7) y
C13 Co1 P4 . . 83.39(18) y
P2 Co1 P4 . . 96.24(6) y
P1 Co1 P4 . . 119.14(8) y
C13 Co1 P3 . . 84.66(19) y
P2 Co1 P3 . . 94.75(7) y
P1 Co1 P3 . . 118.05(8) y
P4 Co1 P3 . . 119.55(8) y
C2 P1 C3 . . 98.9(6) ?
C2 P1 C1 . . 97.5(5) ?
C3 P1 C1 . . 98.0(5) ?
C2 P1 Co1 . . 114.9(3) ?
C3 P1 Co1 . . 115.5(4) ?
C1 P1 Co1 . . 127.1(3) ?
C6 P2 C5 . . 97.6(4) ?
C6 P2 C4 . . 99.2(4) ?
C5 P2 C4 . . 100.1(4) ?
C6 P2 Co1 . . 119.5(3) ?
C5 P2 Co1 . . 118.6(3) ?
C4 P2 Co1 . . 117.9(3) ?
C9 P3 C8 . . 97.9(3) ?
C9 P3 C7 . . 96.9(4) ?
C8 P3 C7 . . 96.1(4) ?
C9 P3 Co1 . . 125.8(2) ?
C8 P3 Co1 . . 119.0(2) ?
C7 P3 Co1 . . 115.3(2) ?
C12 P4 C10 . . 96.9(5) ?
C12 P4 C11 . . 100.4(6) ?
C10 P4 C11 . . 96.6(5) ?
C12 P4 Co1 . . 115.5(4) ?
C10 P4 Co1 . . 127.6(3) ?
C11 P4 Co1 . . 115.0(4) ?
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 P1 . 1.863(8) ?
C1 H1A . 0.9600 ?
C1 H1B . 0.9600 ?
C1 H1C . 0.9600 ?
C2 P1 . 1.840(10) ?
C2 H2A . 0.9600 ?
C2 H2B . 0.9600 ?
C2 H2C . 0.9600 ?
C3 P1 . 1.850(9) ?
C3 H3A . 0.9600 ?
C3 H3B . 0.9600 ?
C3 H3C . 0.9600 ?
C4 P2 . 1.855(7) ?
C4 H4A . 0.9600 ?
C4 H4B . 0.9600 ?
C4 H4C . 0.9600 ?
C5 P2 . 1.850(7) ?
C5 H5A . 0.9600 ?
C5 H5B . 0.9600 ?
C5 H5C . 0.9600 ?
C6 P2 . 1.847(7) ?
C6 H6A . 0.9600 ?
C6 H6B . 0.9600 ?
C6 H6C . 0.9600 ?
C7 P3 . 1.881(8) ?
C7 H7A . 0.9600 ?
C7 H7B . 0.9600 ?
C7 H7C . 0.9600 ?
C8 P3 . 1.820(7) ?
C8 H8A . 0.9600 ?
C8 H8B . 0.9600 ?
C8 H8C . 0.9600 ?
C9 P3 . 1.816(7) ?
C9 H9A . 0.9600 ?
C9 H9B . 0.9600 ?
C9 H9C . 0.9600 ?
C10 P4 . 1.858(9) ?
C10 H10A . 0.9600 ?
C10 H10B . 0.9600 ?
C10 H10C . 0.9600 ?
C11 P4 . 1.866(11) ?
C11 H11A . 0.9600 ?
C11 H11B . 0.9600 ?
C11 H11C . 0.9600 ?
C12 P4 . 1.833(10) ?
C12 H12A . 0.9600 ?
C12 H12B . 0.9600 ?
C12 H12C . 0.9600 ?
C13 N1 . 1.166(7) y
Co1 C13 . 1.896(5) y
Co1 P2 . 2.2018(15) y
Co1 P1 . 2.2082(17) y
Co1 P4 . 2.2115(17) y
Co1 P3 . 2.2272(17) y
