#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/28/4322846.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_4322846
loop_
_publ_author_name
'Masaaki Ohba'
'Naoki Usuki'
'Nobuo Fukita'
'Hisashi Ōkawa'
_publ_section_title
;
 Structure and Magnetic Properties of One-Dimensional
 PPh4[Ni(pn)2][M(CN)6].H2O (M = Fe, Cr, Co) Bimetallic Assemblies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3349
_journal_page_last               3354
_journal_paper_doi               10.1021/ic9704748
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C36 H42 Co N10 Ni O P'
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      13
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_audit_creation_date             'Sun Apr 13 14:46:18 1997'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 99.840(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2.00
_cell_length_a                   12.971(1)
_cell_length_b                   8.437(1)
_cell_length_c                   17.118(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    20.0
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      29.56
_cell_volume                     1845.8(3)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan: PROCESS (MSC)'
_computing_publication_material  'teXsan: FINISH (MSC)'
_computing_structure_refinement  'teXsan: LS (MSC)'
_diffrn_ambient_temperature      20.0
_diffrn_measurement_device       AFC7R
_diffrn_measurement_method       'omega/2-theta scans'
_diffrn_orient_matrix_UB_11      -0.06301
_diffrn_orient_matrix_UB_12      0.03412
_diffrn_orient_matrix_UB_13      -0.03844
_diffrn_orient_matrix_UB_21      0.03063
_diffrn_orient_matrix_UB_22      0.10842
_diffrn_orient_matrix_UB_23      -0.00188
_diffrn_orient_matrix_UB_31      0.03485
_diffrn_orient_matrix_UB_32      -0.03360
_diffrn_orient_matrix_UB_33      -0.04510
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  2.33
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3669
_diffrn_reflns_theta_max         25.0002
_diffrn_standards_decay_%        -0.73
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu_cm 10.469
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.905
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_description       trigonal
_exptl_crystal_F_000             812.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         -0.59790
_refine_diff_density_min         0.74390
_refine_ls_extinction_coef       0.00000
_refine_ls_extinction_method     Zachariasen_type_2_Gaussian_isotropic
_refine_ls_goodness_of_fit_obs   7.090
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         2946
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0730
_refine_ls_shift/esd_max         3.8510
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0730
_cod_data_source_file            ic9704748_3.cif
_cod_data_source_block           PPh4[Ni(pn)2][Co(CN)6].H2O(3)
_cod_original_cell_volume        1845.7(3)
_cod_original_sg_symbol_H-M      'P 2/c '
_cod_original_formula_sum        'C36 H42 N10 O P Co Ni'
_cod_database_code               4322846
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
'   -x,   +y,1/2-z'
'   -x,   -y,   -z'
'   +x,   -y,1/2+z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
Ni 0.0000 0.0000 0.0000 0.0283(3) Uij ? ?
Co 0.0000 0.3243(1) 0.2500 0.0266(3) Uij ? ?
P1 0.5000 0.0646(3) 0.2500 0.0381(6) Uij ? ?
O1 0.8889(8) 0.490(1) 0.4996(6) 0.076(4) Uij ? ?
N1 0.0317(4) 0.0939(6) 0.1183(2) 0.035(1) Uij ? ?
N2 -0.2299(4) 0.3183(7) 0.1700(3) 0.050(2) Uij ? ?
N3 0.0425(5) 0.5859(8) 0.1385(3) 0.080(2) Uij ? ?
N4 -0.1256(3) 0.1586(5) -0.0269(3) 0.035(1) Uij ? ?
N5 -0.1130(4) -0.1458(6) 0.0370(3) 0.042(1) Uij ? ?
C1 0.0236(4) 0.1718(6) 0.1700(3) 0.027(1) Uij ? ?
C2 -0.1448(5) 0.3218(7) 0.2006(3) 0.035(2) Uij ? ?
C3 0.0279(5) 0.4883(7) 0.1791(3) 0.041(2) Uij ? ?
C4 -0.2213(5) 0.0672(8) -0.0287(4) 0.052(2) Uij ? ?
C5 -0.3184(5) 0.1669(9) -0.0345(4) 0.057(2) Uij ? ?
C6 -0.2063(5) -0.0460(9) 0.0384(4) 0.060(2) Uij ? ?
C7 0.3974(4) -0.0649(7) 0.2725(3) 0.039(2) Uij ? ?
C8 0.4251(5) -0.2068(8) 0.3117(4) 0.049(2) Uij ? ?
C9 0.3480(5) -0.3125(8) 0.3232(4) 0.052(2) Uij ? ?
C10 0.2447(5) -0.2806(8) 0.2958(4) 0.052(2) Uij ? ?
C11 0.2169(5) -0.1377(9) 0.2591(4) 0.052(2) Uij ? ?
C12 0.2923(5) -0.0283(7) 0.2467(3) 0.042(2) Uij ? ?
C13 0.4505(5) 0.1952(7) 0.1680(3) 0.040(2) Uij ? ?
C14 0.3761(6) 0.3067(8) 0.1795(4) 0.057(2) Uij ? ?
C15 0.3357(5) 0.4065(8) 0.1181(4) 0.060(2) Uij ? ?
C16 0.3729(6) 0.3988(9) 0.0475(4) 0.061(2) Uij ? ?
C17 0.4504(5) 0.2923(9) 0.0387(4) 0.055(2) Uij ? ?
C18 0.4898(5) 0.1887(8) 0.0983(4) 0.046(2) Uij ? ?
H1 -0.1239 0.2522 0.0122 0.0429 Uij ? ?
H2 -0.0983 0.1614 -0.0769 0.0429 Uij ? ?
H3 -0.2275 -0.0147 -0.0759 0.0429 Uij ? ?
H4 -0.3198 0.2453 0.0161 0.0429 Uij ? ?
H5 -0.3177 0.2081 -0.0772 0.0429 Uij ? ?
H6 -0.3797 0.1016 -0.0356 0.0429 Uij ? ?
H7 -0.1996 0.0335 0.0884 0.0429 Uij ? ?
H8 -0.2777 -0.1162 0.0210 0.0429 Uij ? ?
H9 -0.0973 -0.1958 0.0855 0.0429 Uij ? ?
H10 -0.1287 -0.2300 0.0056 0.0429 Uij ? ?
H11 0.4958 -0.2337 0.3335 0.0429 Uij ? ?
H12 0.3726 -0.4201 0.3482 0.0429 Uij ? ?
H13 0.1892 -0.3602 0.3096 0.0429 Uij ? ?
H14 0.1433 -0.1133 0.2374 0.0429 Uij ? ?
H15 0.2682 0.0633 0.2034 0.0429 Uij ? ?
H16 0.3523 0.3196 0.2302 0.0429 Uij ? ?
H17 0.2761 0.4839 0.1250 0.0429 Uij ? ?
H18 0.3502 0.4748 0.0040 0.0429 Uij ? ?
H19 0.4751 0.2874 -0.0131 0.0429 Uij ? ?
H20 0.5512 0.1147 0.0897 0.0429 Uij ? ?
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0 72 0.003 0.002 'International Tables'
H 0 84 0.000 0.000 'International Tables'
N 0 20 0.006 0.003 'International Tables'
O 0 2 0.011 0.006 'International Tables'
P 0 2 0.102 0.094 'International Tables'
Ni 0 2 0.339 1.112 'International Tables'
Co 0 2 0.349 0.972 'International Tables'
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N(1) Ni N(1) 180.0000 ? ? ? yes
N(1) Ni N(4) 89.3(2) ? ? ? yes
N(1) Ni N(4) 90.7(2) ? ? ? yes
N(1) Ni N(5) 87.9(2) ? ? ? yes
N(1) Ni N(5) 92.1(2) ? ? ? yes
N(1) Ni N(4) 90.7(2) ? ? ? yes
N(1) Ni N(4) 89.3(2) ? ? ? yes
N(1) Ni N(5) 92.1(2) ? ? ? yes
N(1) Ni N(5) 87.9(2) ? ? ? yes
N(4) Ni N(4) 180.0000 ? ? ? yes
N(4) Ni N(5) 83.3(2) ? ? ? yes
N(4) Ni N(5) 96.7(2) ? ? ? yes
N(4) Ni N(5) 96.7(2) ? ? ? yes
N(4) Ni N(5) 83.3(2) ? ? ? yes
N(5) Ni N(5) 180.0000 ? ? ? yes
C(1) Co C(1) 97.0(3) ? ? ? yes
C(1) Co C(2) 86.7(2) ? ? ? yes
C(1) Co C(2) 92.5(2) ? ? ? yes
C(1) Co C(3) 87.8(2) ? ? ? yes
C(1) Co C(3) 174.6(2) ? ? ? yes
C(1) Co C(2) 92.5(2) ? ? ? yes
C(1) Co C(2) 86.7(2) ? ? ? yes
C(1) Co C(3) 174.6(2) ? ? ? yes
C(1) Co C(3) 87.8(2) ? ? ? yes
C(2) Co C(2) 178.8(3) ? ? ? yes
C(2) Co C(3) 90.3(2) ? ? ? yes
C(2) Co C(3) 90.6(2) ? ? ? yes
C(2) Co C(3) 90.6(2) ? ? ? yes
C(2) Co C(3) 90.3(2) ? ? ? yes
C(3) Co C(3) 87.5(4) ? ? ? yes
C(7) P(1) C(7) 105.9(4) ? ? ? yes
C(7) P(1) C(13) 110.8(3) ? ? ? yes
C(7) P(1) C(13) 112.2(3) ? ? ? yes
C(7) P(1) C(13) 112.2(3) ? ? ? yes
C(7) P(1) C(13) 110.8(3) ? ? ? yes
C(13) P(1) C(13) 105.1(4) ? ? ? yes
Ni N(1) C(1) 158.7(4) ? ? ? yes
Ni N(4) C(4) 107.1(4) ? ? ? yes
Ni N(4) H(1) 114.5408 ? ? ? no
Ni N(4) H(2) 79.8866 ? ? ? no
C(4) N(4) H(1) 110.0121 ? ? ? no
C(4) N(4) H(2) 115.2761 ? ? ? no
H(1) N(4) H(2) 125.2189 ? ? ? no
Ni N(5) C(6) 106.7(4) ? ? ? yes
Ni N(5) H(9) 118.8009 ? ? ? no
Ni N(5) H(10) 112.6169 ? ? ? no
C(6) N(5) H(9) 107.5397 ? ? ? no
C(6) N(5) H(10) 111.1723 ? ? ? no
H(9) N(5) H(10) 99.8344 ? ? ? no
Co C(1) N(1) 172.9(5) ? ? ? yes
Co C(2) N(2) 178.4(5) ? ? ? yes
Co C(3) N(3) 178.4(7) ? ? ? yes
N(4) C(4) C(5) 113.9(5) ? ? ? yes
N(4) C(4) C(6) 109.0(5) ? ? ? yes
N(4) C(4) H(3) 108.4554 ? ? ? no
C(5) C(4) C(6) 114.2(6) ? ? ? yes
C(5) C(4) H(3) 111.2380 ? ? ? no
C(6) C(4) H(3) 98.8374 ? ? ? no
C(4) C(5) H(4) 114.4101 ? ? ? no
C(4) C(5) H(5) 99.2649 ? ? ? no
C(4) C(5) H(6) 111.1178 ? ? ? no
H(4) C(5) H(5) 117.3526 ? ? ? no
H(4) C(5) H(6) 103.6475 ? ? ? no
H(5) C(5) H(6) 111.3082 ? ? ? no
N(5) C(6) C(4) 110.7(5) ? ? ? yes
N(5) C(6) H(7) 114.3486 ? ? ? no
N(5) C(6) H(8) 110.0773 ? ? ? no
C(4) C(6) H(7) 101.3161 ? ? ? no
C(4) C(6) H(8) 98.2979 ? ? ? no
H(7) C(6) H(8) 120.0865 ? ? ? no
P(1) C(7) C(8) 118.9(5) ? ? ? yes
P(1) C(7) C(12) 120.9(5) ? ? ? yes
C(8) C(7) C(12) 120.1(6) ? ? ? yes
C(7) C(8) C(9) 119.5(6) ? ? ? yes
C(7) C(8) H(11) 123.0435 ? ? ? no
C(9) C(8) H(11) 117.4289 ? ? ? no
C(8) C(9) C(10) 121.0(6) ? ? ? yes
C(8) C(9) H(12) 116.6476 ? ? ? no
C(10) C(9) H(12) 122.0434 ? ? ? no
C(9) C(10) C(11) 119.5(6) ? ? ? yes
C(9) C(10) H(13) 118.0365 ? ? ? no
C(11) C(10) H(13) 122.0004 ? ? ? no
C(10) C(11) C(12) 121.0(6) ? ? ? yes
C(10) C(11) H(14) 121.1200 ? ? ? no
C(12) C(11) H(14) 117.7579 ? ? ? no
C(7) C(12) C(11) 118.8(6) ? ? ? yes
C(7) C(12) H(15) 121.8647 ? ? ? no
C(11) C(12) H(15) 116.9085 ? ? ? no
P(1) C(13) C(14) 117.8(5) ? ? ? yes
P(1) C(13) C(18) 120.8(5) ? ? ? yes
C(14) C(13) C(18) 121.3(6) ? ? ? yes
C(13) C(14) C(15) 119.4(6) ? ? ? yes
C(13) C(14) H(16) 122.3060 ? ? ? no
C(15) C(14) H(16) 118.2646 ? ? ? no
C(14) C(15) C(16) 119.7(6) ? ? ? yes
C(14) C(15) H(17) 119.4935 ? ? ? no
C(16) C(15) H(17) 120.8096 ? ? ? no
C(15) C(16) C(17) 119.9(6) ? ? ? yes
C(15) C(16) H(18) 121.7235 ? ? ? no
C(17) C(16) H(18) 118.0969 ? ? ? no
C(16) C(17) C(18) 121.3(6) ? ? ? yes
C(16) C(17) H(19) 118.5109 ? ? ? no
C(18) C(17) H(19) 120.0710 ? ? ? no
C(13) C(18) C(17) 118.3(6) ? ? ? yes
C(13) C(18) H(20) 123.4612 ? ? ? no
C(17) C(18) H(20) 118.1432 ? ? ? no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni N(1) 2.147(4) ? ? yes
Ni N(1) 2.147(4) ? ? yes
Ni N(4) 2.098(4) ? ? yes
Ni N(4) 2.098(4) ? ? yes
Ni N(5) 2.093(4) ? ? yes
Ni N(5) 2.093(4) ? ? yes
Co C(1) 1.941(5) ? ? yes
Co C(1) 1.941(5) ? ? yes
Co C(2) 1.924(6) ? ? yes
Co C(2) 1.924(6) ? ? yes
Co C(3) 1.916(5) ? ? yes
Co C(3) 1.916(5) ? ? yes
P(1) C(7) 1.813(6) ? ? yes
P(1) C(7) 1.813(6) ? ? yes
P(1) C(13) 1.813(6) ? ? yes
P(1) C(13) 1.813(6) ? ? yes
N(1) C(1) 1.122(6) ? ? yes
N(2) C(2) 1.137(7) ? ? yes
N(3) C(3) 1.114(7) ? ? yes
N(4) C(4) 1.457(7) ? ? yes
N(4) H(1) 1.0328 ? ? no
N(4) H(2) 0.9811 ? ? no
N(5) C(6) 1.477(8) ? ? yes
N(5) H(9) 0.9224 ? ? no
N(5) H(10) 0.8925 ? ? no
C(4) C(5) 1.504(8) ? ? yes
C(4) C(6) 1.481(9) ? ? yes
C(4) H(3) 1.0554 ? ? no
C(5) H(4) 1.0928 ? ? no
C(5) H(5) 0.8109 ? ? no
C(5) H(6) 0.9655 ? ? no
C(6) H(7) 1.0798 ? ? no
C(6) H(8) 1.0970 ? ? no
C(7) C(8) 1.390(8) ? ? yes
C(7) C(12) 1.393(8) ? ? yes
C(8) C(9) 1.379(8) ? ? yes
C(8) H(11) 0.9556 ? ? no
C(9) C(10) 1.368(9) ? ? yes
C(9) H(12) 1.0305 ? ? no
C(10) C(11) 1.378(9) ? ? yes
C(10) H(13) 1.0413 ? ? no
C(11) C(12) 1.388(8) ? ? yes
C(11) H(14) 0.9852 ? ? no
C(12) H(15) 1.0801 ? ? no
C(13) C(14) 1.386(8) ? ? yes
C(13) C(18) 1.376(8) ? ? yes
C(14) C(15) 1.378(9) ? ? yes
C(14) H(16) 0.9769 ? ? no
C(15) C(16) 1.378(9) ? ? yes
C(15) H(17) 1.0340 ? ? no
C(16) C(17) 1.375(9) ? ? yes
C(16) H(18) 0.9887 ? ? no
C(17) C(18) 1.374(9) ? ? yes
C(17) H(19) 0.9928 ? ? no
C(18) H(20) 1.0423 ? ? no
