#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/28/4322844.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_4322844
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 Fe 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 10:13:12 1997'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 99.96(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2.00
_cell_length_a                   12.958(3)
_cell_length_b                   8.437(3)
_cell_length_c                   17.250(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    20.0
_cell_measurement_theta_max      29.71
_cell_measurement_theta_min      28.66
_cell_volume                     1857.5(8)
_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      -0.03537
_diffrn_orient_matrix_UB_12      0.10524
_diffrn_orient_matrix_UB_13      -0.00979
_diffrn_orient_matrix_UB_21      0.01348
_diffrn_orient_matrix_UB_22      0.02193
_diffrn_orient_matrix_UB_23      0.05784
_diffrn_orient_matrix_UB_31      0.06861
_diffrn_orient_matrix_UB_32      0.04994
_diffrn_orient_matrix_UB_33      -0.00478
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  1.15
_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       -19
_diffrn_reflns_number            3692
_diffrn_reflns_theta_max         25.0075
_diffrn_standards_decay_%        -0.01
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu_cm 9.838
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.896
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             810.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         -1.02400
_refine_diff_density_min         1.01910
_refine_ls_extinction_coef       0.00000
_refine_ls_extinction_method     Zachariasen_type_2_Gaussian_isotropic
_refine_ls_goodness_of_fit_obs   4.400
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         2232
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0750
_refine_ls_shift/esd_max         1.6280
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0640
_cod_data_source_file            ic9704748_1.cif
_cod_data_source_block           Pph4[Ni(pn)2][Fe(CN)6].H2O(1)
_cod_original_cell_volume        1857.4(7)
_cod_original_sg_symbol_H-M      'P 2/c '
_cod_original_formula_sum        'C36 H42 N10 O P Fe Ni'
_cod_database_code               4322844
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 0.0319 Uij ? ?
Fe 0.0000 0.3263(2) 0.2500 0.0309 Uij ? ?
P1 0.5000 0.0690(3) 0.2500 0.0421 Uij ? ?
O1 0.898(1) 0.493(1) 0.4969(7) 0.0756 Uij ? ?
N1 0.0349(5) 0.0951(7) 0.1173(3) 0.0403 Uij ? ?
N2 -0.2325(6) 0.3208(8) 0.1678(4) 0.0543 Uij ? ?
N3 0.0487(8) 0.5894(9) 0.1368(4) 0.0903 Uij ? ?
N4 -0.1234(6) 0.1552(7) -0.0261(3) 0.0508 Uij ? ?
N5 -0.1105(6) -0.1465(7) 0.0360(3) 0.0482 Uij ? ?
C1 0.0259(7) 0.1735(8) 0.1699(4) 0.0357 Uij ? ?
C2 -0.1479(7) 0.3237(8) 0.1990(4) 0.0327 Uij ? ?
C3 0.0309(8) 0.4915(9) 0.1784(4) 0.0537 Uij ? ?
C4 -0.2192(8) 0.0677(10) -0.0275(5) 0.0573 Uij ? ?
C5 -0.3226(9) 0.158(1) -0.0325(5) 0.0750 Uij ? ?
C6 -0.210(1) -0.053(1) 0.0365(5) 0.0861 Uij ? ?
C7 0.3946(7) -0.0580(8) 0.2732(4) 0.0405 Uij ? ?
C8 0.4243(8) -0.2033(9) 0.3125(4) 0.0561 Uij ? ?
C9 0.3464(8) -0.3074(10) 0.3238(4) 0.0500 Uij ? ?
C10 0.2488(8) -0.2752(10) 0.2945(5) 0.0553 Uij ? ?
C11 0.2203(7) -0.135(1) 0.2572(5) 0.0510 Uij ? ?
C12 0.2923(8) -0.0266(9) 0.2462(4) 0.0472 Uij ? ?
C13 0.4516(8) 0.2003(8) 0.1684(4) 0.0458 Uij ? ?
C14 0.3736(9) 0.3098(9) 0.1812(5) 0.0654 Uij ? ?
C15 0.333(1) 0.4106(10) 0.1187(5) 0.0804 Uij ? ?
C16 0.3764(10) 0.399(1) 0.0474(5) 0.0730 Uij ? ?
C17 0.4536(8) 0.296(1) 0.0389(4) 0.0610 Uij ? ?
C18 0.4893(7) 0.1941(9) 0.0990(4) 0.0499 Uij ? ?
H1 -0.1745 0.2195 0.0181 0.0499 Uij ? ?
H2 -0.0957 0.1959 -0.0781 0.0775 Uij ? ?
H3 -0.2255 0.0077 -0.0742 0.0707 Uij ? ?
H4 -0.3208 0.2375 -0.0735 0.0815 Uij ? ?
H5 -0.3241 0.2069 0.0147 0.0815 Uij ? ?
H6 -0.3767 0.0881 -0.0487 0.0815 Uij ? ?
H7 -0.2056 -0.0095 0.0862 0.0926 Uij ? ?
H8 -0.2658 -0.1285 0.0263 0.0682 Uij ? ?
H9 -0.1230 -0.2362 0.0016 0.0585 Uij ? ?
H10 -0.0837 -0.1862 0.0882 0.0775 Uij ? ?
H11 0.4963 -0.2274 0.3309 0.0738 Uij ? ?
H12 0.3654 -0.4016 0.3521 0.0631 Uij ? ?
H13 0.1964 -0.3522 0.3008 0.0662 Uij ? ?
H14 0.1482 -0.1122 0.2383 0.0671 Uij ? ?
H15 0.2731 0.0705 0.2207 0.0633 Uij ? ?
H16 0.3543 0.3169 0.2301 0.0917 Uij ? ?
H17 0.2811 0.4846 0.1244 0.1001 Uij ? ?
H18 0.3493 0.4676 0.0048 0.0799 Uij ? ?
H19 0.4809 0.2953 -0.0077 0.0693 Uij ? ?
H20 0.5406 0.1187 0.0929 0.0574 Uij ? ?
H21 0.8151 0.4913 0.5242 0.0499 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'
Fe 0 2 0.346 0.844 'International Tables'
Ni 0 2 0.339 1.112 '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) 89.9(3) ? ? ? yes
N(1) Ni N(4) 90.1(3) ? ? ? yes
N(1) Ni N(5) 89.1(3) ? ? ? yes
N(1) Ni N(5) 90.9(3) ? ? ? yes
N(1) Ni N(4) 90.1(3) ? ? ? yes
N(1) Ni N(4) 89.9(3) ? ? ? yes
N(1) Ni N(5) 90.9(3) ? ? ? yes
N(1) Ni N(5) 89.1(3) ? ? ? yes
N(4) Ni N(4) 180.0000 ? ? ? yes
N(4) Ni N(5) 83.5(3) ? ? ? yes
N(4) Ni N(5) 96.5(3) ? ? ? yes
N(4) Ni N(5) 96.5(3) ? ? ? yes
N(4) Ni N(5) 83.5(3) ? ? ? yes
N(5) Ni N(5) 180.0000 ? ? ? yes
C(1) Fe C(1) 98.0(5) ? ? ? yes
C(1) Fe C(2) 87.0(4) ? ? ? yes
C(1) Fe C(2) 92.3(4) ? ? ? yes
C(1) Fe C(3) 86.4(4) ? ? ? yes
C(1) Fe C(3) 174.8(3) ? ? ? yes
C(1) Fe C(2) 92.3(4) ? ? ? yes
C(1) Fe C(2) 87.0(4) ? ? ? yes
C(1) Fe C(3) 174.8(3) ? ? ? yes
C(1) Fe C(3) 86.4(4) ? ? ? yes
C(2) Fe C(2) 179.0(5) ? ? ? yes
C(2) Fe C(3) 90.7(4) ? ? ? yes
C(2) Fe C(3) 90.1(4) ? ? ? yes
C(2) Fe C(3) 90.1(4) ? ? ? yes
C(2) Fe C(3) 90.7(4) ? ? ? yes
C(3) Fe C(3) 89.3(6) ? ? ? yes
C(7) P(1) C(7) 108.0(6) ? ? ? yes
C(7) P(1) C(13) 110.9(4) ? ? ? yes
C(7) P(1) C(13) 111.0(4) ? ? ? yes
C(7) P(1) C(13) 111.0(4) ? ? ? yes
C(7) P(1) C(13) 110.9(4) ? ? ? yes
C(13) P(1) C(13) 105.1(6) ? ? ? yes
Ni N(1) C(1) 157.9(7) ? ? ? yes
Ni N(4) C(4) 108.2(6) ? ? ? yes
Ni N(4) H(1) 129.3112 ? ? ? no
Ni N(4) H(2) 91.0263 ? ? ? no
C(4) N(4) H(1) 72.0450 ? ? ? no
C(4) N(4) H(2) 124.3513 ? ? ? no
H(1) N(4) H(2) 132.1049 ? ? ? no
Ni N(5) C(6) 109.8(6) ? ? ? yes
Ni N(5) H(9) 109.9795 ? ? ? no
Ni N(5) H(10) 109.8181 ? ? ? no
C(6) N(5) H(9) 110.7649 ? ? ? no
C(6) N(5) H(10) 109.8188 ? ? ? no
H(9) N(5) H(10) 106.5968 ? ? ? no
Fe C(1) N(1) 172.6(8) ? ? ? yes
Fe C(2) N(2) 179.2(8) ? ? ? yes
Fe C(3) N(3) 178(1) ? ? ? yes
N(4) C(4) C(5) 118.1(9) ? ? ? yes
N(4) C(4) C(6) 113.1(9) ? ? ? yes
N(4) C(4) H(3) 104.3662 ? ? ? no
C(5) C(4) C(6) 110(1) ? ? ? yes
C(5) C(4) H(3) 104.7364 ? ? ? no
C(6) C(4) H(3) 104.6463 ? ? ? no
C(4) C(5) H(4) 108.1696 ? ? ? no
C(4) C(5) H(5) 109.7614 ? ? ? no
C(4) C(5) H(6) 109.1363 ? ? ? no
H(4) C(5) H(5) 109.8454 ? ? ? no
H(4) C(5) H(6) 109.4377 ? ? ? no
H(5) C(5) H(6) 110.4505 ? ? ? no
N(5) C(6) C(4) 106(1) ? ? ? yes
N(5) C(6) H(7) 106.9517 ? ? ? no
N(5) C(6) H(8) 106.0552 ? ? ? no
C(4) C(6) H(7) 113.2396 ? ? ? no
C(4) C(6) H(8) 111.1532 ? ? ? no
H(7) C(6) H(8) 112.0806 ? ? ? no
P(1) C(7) C(8) 117.8(8) ? ? ? yes
P(1) C(7) C(12) 122.5(7) ? ? ? yes
C(8) C(7) C(12) 119.3(9) ? ? ? yes
C(7) C(8) C(9) 118(1) ? ? ? yes
C(7) C(8) H(11) 120.5600 ? ? ? no
C(9) C(8) H(11) 120.8076 ? ? ? no
C(8) C(9) C(10) 120.7(10) ? ? ? yes
C(8) C(9) H(12) 119.2680 ? ? ? no
C(10) C(9) H(12) 120.0262 ? ? ? no
C(9) C(10) C(11) 121(1) ? ? ? yes
C(9) C(10) H(13) 119.5621 ? ? ? no
C(11) C(10) H(13) 119.3673 ? ? ? no
C(10) C(11) C(12) 120(1) ? ? ? yes
C(10) C(11) H(14) 120.2068 ? ? ? no
C(12) C(11) H(14) 119.4201 ? ? ? no
C(7) C(12) C(11) 119.8(9) ? ? ? yes
C(7) C(12) H(15) 119.4574 ? ? ? no
C(11) C(12) H(15) 120.7106 ? ? ? no
P(1) C(13) C(14) 116.4(7) ? ? ? yes
P(1) C(13) C(18) 122.4(8) ? ? ? yes
C(14) C(13) C(18) 121.2(8) ? ? ? yes
C(13) C(14) C(15) 118(1) ? ? ? yes
C(13) C(14) H(16) 120.1284 ? ? ? no
C(15) C(14) H(16) 121.2325 ? ? ? no
C(14) C(15) C(16) 116(1) ? ? ? yes
C(14) C(15) H(17) 120.9114 ? ? ? no
C(16) C(15) H(17) 122.5829 ? ? ? no
C(15) C(16) C(17) 122.6(10) ? ? ? yes
C(15) C(16) H(18) 116.2625 ? ? ? no
C(17) C(16) H(18) 121.0870 ? ? ? no
C(16) C(17) C(18) 119.4(10) ? ? ? yes
C(16) C(17) H(19) 119.2849 ? ? ? no
C(18) C(17) H(19) 121.2814 ? ? ? no
C(13) C(18) C(17) 121.5(10) ? ? ? yes
C(13) C(18) H(20) 118.6134 ? ? ? no
C(17) C(18) H(20) 119.8841 ? ? ? 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) 2.151(5) ? ? yes
Ni N(1) 2.151(5) ? ? yes
Ni N(4) 2.056(7) ? ? yes
Ni N(4) 2.056(7) ? ? yes
Ni N(5) 2.067(7) ? ? yes
Ni N(5) 2.067(7) ? ? yes
Fe C(1) 1.960(7) ? ? yes
Fe C(1) 1.960(7) ? ? yes
Fe C(2) 1.966(8) ? ? yes
Fe C(2) 1.966(8) ? ? yes
Fe C(3) 1.949(8) ? ? yes
Fe C(3) 1.949(8) ? ? yes
P(1) C(7) 1.834(8) ? ? yes
P(1) C(7) 1.834(8) ? ? yes
P(1) C(13) 1.815(7) ? ? yes
P(1) C(13) 1.815(7) ? ? yes
O(1) H(21) 1.2492 ? ? no
N(1) C(1) 1.145(8) ? ? yes
N(2) C(2) 1.135(10) ? ? yes
N(3) C(3) 1.145(10) ? ? yes
N(4) C(4) 1.44(1) ? ? yes
N(4) H(1) 1.2198 ? ? no
N(4) H(2) 1.0788 ? ? no
N(5) C(6) 1.52(1) ? ? yes
N(5) H(9) 0.9584 ? ? no
N(5) H(10) 0.9661 ? ? no
C(4) C(5) 1.53(1) ? ? yes
C(4) C(6) 1.49(1) ? ? yes
C(4) H(3) 0.9423 ? ? no
C(5) H(4) 0.9766 ? ? no
C(5) H(5) 0.9147 ? ? no
C(5) H(6) 0.9234 ? ? no
C(6) H(7) 0.9258 ? ? no
C(6) H(8) 0.9524 ? ? no
C(7) C(8) 1.421(10) ? ? yes
C(7) C(12) 1.35(1) ? ? yes
C(8) C(9) 1.38(1) ? ? yes
C(8) H(11) 0.9548 ? ? no
C(9) C(10) 1.31(1) ? ? yes
C(9) H(12) 0.9426 ? ? no
C(10) C(11) 1.37(1) ? ? yes
C(10) H(13) 0.9594 ? ? no
C(11) C(12) 1.34(1) ? ? yes
C(11) H(14) 0.9541 ? ? no
C(12) H(15) 0.9426 ? ? no
C(13) C(14) 1.42(1) ? ? yes
C(13) C(18) 1.37(1) ? ? yes
C(14) C(15) 1.40(1) ? ? yes
C(14) H(16) 0.9223 ? ? no
C(15) C(16) 1.44(1) ? ? yes
C(15) H(17) 0.9326 ? ? no
C(16) C(17) 1.35(1) ? ? yes
C(16) H(18) 0.9544 ? ? no
C(17) C(18) 1.367(10) ? ? yes
C(17) H(19) 0.9321 ? ? no
C(18) H(20) 0.9397 ? ? no
