#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/28/4322845.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_4322845
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 Cr 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             'Thu Apr 24 10:10:48 1997'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 100.15(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2.00
_cell_length_a                   12.927(2)
_cell_length_b                   8.454(2)
_cell_length_c                   17.564(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    20.0
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      29.49
_cell_volume                     1889.4(6)
_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      -0.00456
_diffrn_orient_matrix_UB_12      -0.05124
_diffrn_orient_matrix_UB_13      0.05062
_diffrn_orient_matrix_UB_21      0.07840
_diffrn_orient_matrix_UB_22      -0.00704
_diffrn_orient_matrix_UB_23      0.01221
_diffrn_orient_matrix_UB_31      0.00299
_diffrn_orient_matrix_UB_32      0.10638
_diffrn_orient_matrix_UB_33      0.02519
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  2.90
_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       19
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3747
_diffrn_reflns_theta_max         25.0219
_diffrn_standards_decay_%        -0.12
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu_cm 8.710
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             806.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         -0.39150
_refine_diff_density_min         0.51890
_refine_ls_extinction_coef       2.06461
_refine_ls_extinction_method     Zachariasen_type_2_Gaussian_isotropic
_refine_ls_goodness_of_fit_obs   3.210
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         2775
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0340
_refine_ls_shift/esd_max         0.6000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0260
_cod_data_source_file            ic9704748_2.cif
_cod_data_source_block           PPh4[Ni(pn)2][Cr(CN)6]H2O(2)
_cod_original_cell_volume        1889.5(6)
_cod_original_sg_symbol_H-M      'P 2/c '
_cod_original_formula_sum        'C36 H42 N10 O P Cr Ni'
_cod_database_code               4322845
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 0.0302 Uij ? ?
Cr 0.0000 0.33271(7) 0.2500 0.0282 Uij ? ?
P1 0.5000 0.0797(1) 0.2500 0.0402 Uij ? ?
O1 0.8950(5) 0.4952(8) 0.5004(4) 0.1394 Uij ? ?
N1 0.0339(2) 0.0926(3) 0.1144(1) 0.0414 Uij ? ?
N2 -0.2399(2) 0.3279(3) 0.1605(2) 0.0576 Uij ? ?
N3 0.0527(2) 0.6045(4) 0.1366(2) 0.0862 Uij ? ?
N4 -0.1284(2) 0.1518(3) -0.0243(2) 0.0393 Uij ? ?
N5 -0.1108(2) -0.1512(4) 0.0361(2) 0.0474 Uij ? ?
C1 0.0276(2) 0.1688(3) 0.1674(1) 0.0325 Uij ? ?
C2 -0.1561(2) 0.3299(4) 0.1933(2) 0.0375 Uij ? ?
C3 0.0343(2) 0.5077(4) 0.1766(2) 0.0466 Uij ? ?
C4 -0.2238(2) 0.0596(4) -0.0260(2) 0.0536 Uij ? ?
C5 -0.3221(3) 0.1552(5) -0.0307(3) 0.0598 Uij ? ?
C6 -0.2065(3) -0.0545(5) 0.0382(3) 0.0653 Uij ? ?
C7 0.3980(2) -0.0490(3) 0.2721(2) 0.0394 Uij ? ?
C8 0.4265(3) -0.1882(4) 0.3125(2) 0.0518 Uij ? ?
C9 0.3517(3) -0.2965(4) 0.3245(2) 0.0561 Uij ? ?
C10 0.2473(3) -0.2670(4) 0.2960(2) 0.0544 Uij ? ?
C11 0.2183(3) -0.1301(5) 0.2576(2) 0.0551 Uij ? ?
C12 0.2925(3) -0.0201(4) 0.2446(2) 0.0451 Uij ? ?
C13 0.4502(2) 0.2075(3) 0.1710(2) 0.0408 Uij ? ?
C14 0.3742(3) 0.3195(4) 0.1797(2) 0.0561 Uij ? ?
C15 0.3338(3) 0.4159(4) 0.1189(2) 0.0650 Uij ? ?
C16 0.3700(3) 0.4075(4) 0.0502(2) 0.0627 Uij ? ?
C17 0.4481(3) 0.3018(4) 0.0426(2) 0.0578 Uij ? ?
C18 0.4885(3) 0.2018(4) 0.1022(2) 0.0467 Uij ? ?
H1 -0.127(2) 0.212(4) -0.073(2) 0.09(1) Uij ? ?
H2 -0.121(2) 0.222(3) 0.010(2) 0.04(1) Uij ? ?
H3 -0.231(3) -0.044(5) -0.071(2) 0.16(2) Uij ? ?
H4 -0.335(2) 0.222(4) -0.077(2) 0.08(1) Uij ? ?
H5 -0.311(2) 0.226(4) 0.016(2) 0.08(1) Uij ? ?
H6 -0.379(2) 0.084(3) -0.033(2) 0.07(1) Uij ? ?
H7 -0.199(3) 0.026(5) 0.090(2) 0.16(2) Uij ? ?
H8 -0.268(2) -0.133(4) 0.032(2) 0.08(1) Uij ? ?
H9 -0.131(3) -0.223(4) 0.000(2) 0.08(1) Uij ? ?
H10 -0.085(2) -0.196(4) 0.079(2) 0.07(1) Uij ? ?
H11 0.496(2) -0.214(3) 0.330(1) 0.047(9) Uij ? ?
H12 0.370(2) -0.387(3) 0.348(2) 0.06(1) Uij ? ?
H13 0.203(2) -0.348(4) 0.299(2) 0.08(1) Uij ? ?
H14 0.154(2) -0.111(4) 0.238(2) 0.06(1) Uij ? ?
H15 0.270(2) 0.076(3) 0.223(1) 0.044(9) Uij ? ?
H16 0.355(2) 0.329(3) 0.226(1) 0.054(10) Uij ? ?
H17 0.287(2) 0.486(4) 0.126(2) 0.06(1) Uij ? ?
H18 0.342(2) 0.473(4) 0.010(2) 0.06(1) Uij ? ?
H19 0.470(2) 0.298(3) -0.003(2) 0.050(10) Uij ? ?
H20 0.536(2) 0.130(3) 0.096(1) 0.038(9) 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'
Cr 0 2 0.321 0.624 '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) 89.4(1) ? ? ? yes
N(1) Ni N(4) 90.6(1) ? ? ? yes
N(1) Ni N(5) 88.7(1) ? ? ? yes
N(1) Ni N(5) 91.3(1) ? ? ? yes
N(1) Ni N(4) 90.6(1) ? ? ? yes
N(1) Ni N(4) 89.4(1) ? ? ? yes
N(1) Ni N(5) 91.3(1) ? ? ? yes
N(1) Ni N(5) 88.7(1) ? ? ? yes
N(4) Ni N(4) 180.0000 ? ? ? yes
N(4) Ni N(5) 82.9(1) ? ? ? yes
N(4) Ni N(5) 97.1(1) ? ? ? yes
N(4) Ni N(5) 97.1(1) ? ? ? yes
N(4) Ni N(5) 82.9(1) ? ? ? yes
N(5) Ni N(5) 180.0000 ? ? ? yes
C(1) Cr C(1) 96.6(2) ? ? ? yes
C(1) Cr C(2) 86.0(1) ? ? ? yes
C(1) Cr C(2) 93.1(1) ? ? ? yes
C(1) Cr C(3) 87.7(1) ? ? ? yes
C(1) Cr C(3) 174.7(1) ? ? ? yes
C(1) Cr C(2) 93.1(1) ? ? ? yes
C(1) Cr C(2) 86.0(1) ? ? ? yes
C(1) Cr C(3) 174.7(1) ? ? ? yes
C(1) Cr C(3) 87.7(1) ? ? ? yes
C(2) Cr C(2) 178.7(2) ? ? ? yes
C(2) Cr C(3) 90.4(1) ? ? ? yes
C(2) Cr C(3) 90.6(1) ? ? ? yes
C(2) Cr C(3) 90.6(1) ? ? ? yes
C(2) Cr C(3) 90.4(1) ? ? ? yes
C(3) Cr C(3) 88.3(2) ? ? ? yes
C(7) P(1) C(7) 105.7(2) ? ? ? yes
C(7) P(1) C(13) 110.8(1) ? ? ? yes
C(7) P(1) C(13) 112.0(1) ? ? ? yes
C(7) P(1) C(13) 112.0(1) ? ? ? yes
C(7) P(1) C(13) 110.8(1) ? ? ? yes
C(13) P(1) C(13) 105.6(2) ? ? ? yes
Ni N(1) C(1) 160.2(2) ? ? ? yes
Ni N(4) C(4) 108.4(2) ? ? ? yes
Ni N(4) H(1) 111(1) ? ? ? no
Ni N(4) H(2) 107(1) ? ? ? no
C(4) N(4) H(1) 113(1) ? ? ? no
C(4) N(4) H(2) 112(1) ? ? ? no
H(1) N(4) H(2) 103(2) ? ? ? no
Ni N(5) C(6) 106.7(2) ? ? ? yes
Ni N(5) H(9) 109(2) ? ? ? no
Ni N(5) H(10) 110(2) ? ? ? no
C(6) N(5) H(9) 104(2) ? ? ? no
C(6) N(5) H(10) 114(2) ? ? ? no
H(9) N(5) H(10) 110(3) ? ? ? no
Cr C(1) N(1) 170.0(2) ? ? ? yes
Cr C(2) N(2) 177.9(3) ? ? ? yes
Cr C(3) N(3) 179.5(3) ? ? ? yes
N(4) C(4) C(5) 114.8(3) ? ? ? yes
N(4) C(4) C(6) 108.8(3) ? ? ? yes
N(4) C(4) H(3) 112(1) ? ? ? no
C(5) C(4) C(6) 114.2(3) ? ? ? yes
C(5) C(4) H(3) 113(1) ? ? ? no
C(6) C(4) H(3) 90(1) ? ? ? no
C(4) C(5) H(4) 112(1) ? ? ? no
C(4) C(5) H(5) 106(1) ? ? ? no
C(4) C(5) H(6) 107(1) ? ? ? no
H(4) C(5) H(5) 108(2) ? ? ? no
H(4) C(5) H(6) 108(2) ? ? ? no
H(5) C(5) H(6) 113(2) ? ? ? no
N(5) C(6) C(4) 110.9(3) ? ? ? yes
N(5) C(6) H(7) 113(2) ? ? ? no
N(5) C(6) H(8) 106(1) ? ? ? no
C(4) C(6) H(7) 101(2) ? ? ? no
C(4) C(6) H(8) 109(1) ? ? ? no
H(7) C(6) H(8) 114(2) ? ? ? no
P(1) C(7) C(8) 118.9(2) ? ? ? yes
P(1) C(7) C(12) 122.1(2) ? ? ? yes
C(8) C(7) C(12) 118.8(3) ? ? ? yes
C(7) C(8) C(9) 120.8(3) ? ? ? yes
C(7) C(8) H(11) 121(1) ? ? ? no
C(9) C(8) H(11) 117(1) ? ? ? no
C(8) C(9) C(10) 119.6(4) ? ? ? yes
C(8) C(9) H(12) 120(2) ? ? ? no
C(10) C(9) H(12) 119(1) ? ? ? no
C(9) C(10) C(11) 120.1(4) ? ? ? yes
C(9) C(10) H(13) 115(2) ? ? ? no
C(11) C(10) H(13) 123(2) ? ? ? no
C(10) C(11) C(12) 121.1(4) ? ? ? yes
C(10) C(11) H(14) 121(2) ? ? ? no
C(12) C(11) H(14) 117(2) ? ? ? no
C(7) C(12) C(11) 119.5(3) ? ? ? yes
C(7) C(12) H(15) 120(1) ? ? ? no
C(11) C(12) H(15) 119(1) ? ? ? no
P(1) C(13) C(14) 119.4(2) ? ? ? yes
P(1) C(13) C(18) 121.4(2) ? ? ? yes
C(14) C(13) C(18) 119.1(3) ? ? ? yes
C(13) C(14) C(15) 119.9(3) ? ? ? yes
C(13) C(14) H(16) 118(1) ? ? ? no
C(15) C(14) H(16) 121(1) ? ? ? no
C(14) C(15) C(16) 120.8(4) ? ? ? yes
C(14) C(15) H(17) 118(2) ? ? ? no
C(16) C(15) H(17) 120(2) ? ? ? no
C(15) C(16) C(17) 119.4(4) ? ? ? yes
C(15) C(16) H(18) 119(1) ? ? ? no
C(17) C(16) H(18) 121(1) ? ? ? no
C(16) C(17) C(18) 120.9(3) ? ? ? yes
C(16) C(17) H(19) 117(1) ? ? ? no
C(18) C(17) H(19) 121(1) ? ? ? no
C(13) C(18) C(17) 119.8(3) ? ? ? yes
C(13) C(18) H(20) 119(1) ? ? ? no
C(17) C(18) H(20) 120(1) ? ? ? 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) 2.128(2) ? ? yes
Ni N(1) 2.128(2) ? ? yes
Ni N(4) 2.082(3) ? ? yes
Ni N(4) 2.082(3) ? ? yes
Ni N(5) 2.100(3) ? ? yes
Ni N(5) 2.100(3) ? ? yes
Cr C(1) 2.083(3) ? ? yes
Cr C(1) 2.083(3) ? ? yes
Cr C(2) 2.087(3) ? ? yes
Cr C(2) 2.087(3) ? ? yes
Cr C(3) 2.062(3) ? ? yes
Cr C(3) 2.062(3) ? ? yes
P(1) C(7) 1.804(3) ? ? yes
P(1) C(7) 1.804(3) ? ? yes
P(1) C(13) 1.786(3) ? ? yes
P(1) C(13) 1.786(3) ? ? yes
N(1) C(1) 1.146(3) ? ? yes
N(2) C(2) 1.134(3) ? ? yes
N(3) C(3) 1.131(4) ? ? yes
N(4) C(4) 1.455(4) ? ? yes
N(4) H(1) 1.00(3) ? ? no
N(4) H(2) 0.83(3) ? ? no
N(5) C(6) 1.489(4) ? ? yes
N(5) H(9) 0.88(3) ? ? no
N(5) H(10) 0.86(3) ? ? no
C(4) C(5) 1.495(4) ? ? yes
C(4) C(6) 1.470(4) ? ? yes
C(4) H(3) 1.17(4) ? ? no
C(5) H(4) 0.97(3) ? ? no
C(5) H(5) 1.01(3) ? ? no
C(5) H(6) 0.94(3) ? ? no
C(6) H(7) 1.12(4) ? ? no
C(6) H(8) 1.03(3) ? ? no
C(7) C(8) 1.390(4) ? ? yes
C(7) C(12) 1.387(4) ? ? yes
C(8) C(9) 1.375(4) ? ? yes
C(8) H(11) 0.93(2) ? ? no
C(9) C(10) 1.378(5) ? ? yes
C(9) H(12) 0.88(3) ? ? no
C(10) C(11) 1.358(5) ? ? yes
C(10) H(13) 0.90(3) ? ? no
C(11) C(12) 1.383(4) ? ? yes
C(11) H(14) 0.85(3) ? ? no
C(12) H(15) 0.93(2) ? ? no
C(13) C(14) 1.392(4) ? ? yes
C(13) C(18) 1.386(4) ? ? yes
C(14) C(15) 1.371(4) ? ? yes
C(14) H(16) 0.90(2) ? ? no
C(15) C(16) 1.371(5) ? ? yes
C(15) H(17) 0.86(3) ? ? no
C(16) C(17) 1.372(4) ? ? yes
C(16) H(18) 0.92(3) ? ? no
C(17) C(18) 1.375(4) ? ? yes
C(17) H(19) 0.89(3) ? ? no
C(18) H(20) 0.89(2) ? ? no
