#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/60/4326047.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_4326047
loop_
_publ_author_name
'Mee Chang'
'Atsushi Kobayashi'
'Kiyohiko Nakajima'
'Ho-Chol Chang'
'Masako Kato'
_publ_contact_author_email       akoba@sci.hokudai.ac.jp
_publ_contact_author_fax         +81-11-706-3447
_publ_contact_author_name        'Atsushi Kobayashi'
_publ_contact_author_phone       +81-11-706-3819
_publ_section_title
;
 Dimensionality Control of Vapochromic Hydrogen-Bonded Proton-Transfer
 Assemblies Composed of a Bis(hydrazone)iron(II) Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8308
_journal_page_last               8317
_journal_paper_doi               10.1021/ic2008396
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C52 H52 Cl2 Fe Ho0 N6 O4.25 P2'
_chemical_formula_sum            'C52 H52 Cl2 Fe Ho0 N6 O4.25 P2'
_chemical_formula_weight         1017.69
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 92.300(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.7688(19)
_cell_length_b                   12.2448(7)
_cell_length_c                   19.2175(16)
_cell_measurement_reflns_used    8327
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.1829
_cell_volume                     4883.3(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 14.7059
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku Mecury'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0160
_diffrn_reflns_av_sigmaI/netI    0.0440
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19170
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.33
_exptl_absorpt_coefficient_mu    0.537
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8791
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_description       Block
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.588
_refine_diff_density_min         -0.686
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         5560
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0321
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0476P)²+0.7813P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0902
_refine_ls_wR_factor_ref         0.0933
_reflns_number_gt                4659
_reflns_number_total             5560
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2008396_si_002_3.cif
_cod_data_source_block           '[Fe(Hpbph)2]Cl2'
_cod_original_sg_symbol_Hall     -C2yc
_cod_database_code               4326047
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Fe Fe 0.0000 0.87357(2) 0.7500 0.01142(9) Uani 1 2 d S
P P -0.081473(18) 0.75109(3) 0.74267(2) 0.01304(10) Uani 1 1 d .
Cl Cl 0.10120(2) 1.05302(4) 0.98300(2) 0.03602(13) Uani 1 1 d .
N3 N -0.00512(6) 0.88472(10) 0.85035(7) 0.0141(3) Uani 1 1 d .
C11 C -0.16770(8) 0.66471(14) 0.64208(9) 0.0210(3) Uani 1 1 d .
H11 H -0.1884 0.6366 0.6802 0.025 Uiso 1 1 calc R
C12 C -0.11102(7) 0.72584(13) 0.65338(8) 0.0157(3) Uani 1 1 d .
C14 C -0.19862(7) 0.86417(13) 0.73986(9) 0.0199(3) Uani 1 1 d .
H14 H -0.1905 0.8765 0.6933 0.024 Uiso 1 1 calc R
C13 C -0.15568(7) 0.80099(13) 0.78125(8) 0.0165(3) Uani 1 1 d .
C7 C -0.08123(7) 0.76951(13) 0.59550(8) 0.0170(3) Uani 1 1 d .
C19 C -0.07109(7) 0.61444(13) 0.78110(8) 0.0159(3) Uani 1 1 d .
C10 C -0.19363(8) 0.64511(14) 0.57587(9) 0.0258(4) Uani 1 1 d .
H10 H -0.2314 0.6048 0.5699 0.031 Uiso 1 1 calc R
N1 N 0.06526(6) 0.99339(10) 0.74771(6) 0.0135(3) Uani 1 1 d .
N2 N -0.05151(6) 0.95910(11) 0.86882(7) 0.0189(3) Uani 1 1 d .
H2 H -0.0606 0.9683 0.9117 0.023 Uiso 1 1 calc R
O1 O 0.22666(7) 0.94316(12) 0.92605(8) 0.0413(4) Uani 1 1 d .
C6 C 0.02655(7) 0.84335(13) 0.90422(8) 0.0167(3) Uani 1 1 d .
H6 H 0.0123 0.8637 0.9476 0.020 Uiso 1 1 calc R
C21 C -0.07387(8) 0.41753(14) 0.77481(10) 0.0263(4) Uani 1 1 d .
H21 H -0.0806 0.3543 0.7487 0.032 Uiso 1 1 calc R
C8 C -0.10785(8) 0.74677(14) 0.52833(9) 0.0237(4) Uani 1 1 d .
H8 H -0.0875 0.7737 0.4896 0.028 Uiso 1 1 calc R
C18 C -0.16847(8) 0.78505(15) 0.85113(9) 0.0247(4) Uani 1 1 d .
H18 H -0.1402 0.7440 0.8793 0.030 Uiso 1 1 calc R
C20 C -0.08054(7) 0.51861(13) 0.74277(9) 0.0190(3) Uani 1 1 d .
H20 H -0.0914 0.5225 0.6954 0.023 Uiso 1 1 calc R
C16 C -0.26548(8) 0.89141(15) 0.83758(10) 0.0290(4) Uani 1 1 d .
H16 H -0.3021 0.9211 0.8564 0.035 Uiso 1 1 calc R
C9 C -0.16317(9) 0.68561(15) 0.51863(9) 0.0279(4) Uani 1 1 d .
H9 H -0.1799 0.6717 0.4739 0.033 Uiso 1 1 calc R
C22 C -0.05729(8) 0.40949(15) 0.84514(10) 0.0301(4) Uani 1 1 d .
H22 H -0.0538 0.3415 0.8665 0.036 Uiso 1 1 calc R
C24 C -0.05224(7) 0.60557(14) 0.85183(9) 0.0206(4) Uani 1 1 d .
H24 H -0.0439 0.6684 0.8779 0.025 Uiso 1 1 calc R
C23 C -0.04595(8) 0.50417(15) 0.88318(9) 0.0276(4) Uani 1 1 d .
H23 H -0.0340 0.4995 0.9302 0.033 Uiso 1 1 calc R
C17 C -0.22317(9) 0.83015(16) 0.87893(10) 0.0308(4) Uani 1 1 d .
H17 H -0.2314 0.8191 0.9256 0.037 Uiso 1 1 calc R
C15 C -0.25327(8) 0.90839(14) 0.76843(10) 0.0257(4) Uani 1 1 d .
H15 H -0.2818 0.9497 0.7407 0.031 Uiso 1 1 calc R
C25 C 0.26588(10) 1.03560(19) 0.91720(13) 0.0467(6) Uani 1 1 d .
H25A H 0.2664 1.0792 0.9587 0.070 Uiso 1 1 calc R
H25B H 0.2490 1.0780 0.8786 0.070 Uiso 1 1 calc R
H25C H 0.3089 1.0126 0.9082 0.070 Uiso 1 1 calc R
C5 C 0.08228(7) 1.01724(13) 0.68257(8) 0.0155(3) Uani 1 1 d .
C1 C 0.09201(7) 1.05320(13) 0.80062(8) 0.0177(3) Uani 1 1 d .
H1 H 0.0799 1.0390 0.8458 0.021 Uiso 1 1 calc R
C4 C 0.12798(7) 1.09676(14) 0.66780(9) 0.0205(3) Uani 1 1 d .
H4 H 0.1396 1.1097 0.6223 0.025 Uiso 1 1 calc R
C2 C 0.13638(8) 1.13397(13) 0.79002(9) 0.0222(4) Uani 1 1 d .
H2A H 0.1537 1.1740 0.8274 0.027 Uiso 1 1 calc R
C3 C 0.15519(8) 1.15521(14) 0.72244(9) 0.0233(4) Uani 1 1 d .
H3 H 0.1859 1.2085 0.7145 0.028 Uiso 1 1 calc R
C26 C 0.09407(12) 1.3501(2) 0.94673(13) 0.0544(6) Uani 1 1 d .
H26A H 0.0918 1.3382 0.8968 0.065 Uiso 1 1 calc R
H26B H 0.0958 1.4275 0.9575 0.065 Uiso 1 1 calc R
O2A O 0.1381(2) 1.2935(4) 0.9791(3) 0.074(2) Uiso 0.415(6) 1 d P
O2B O 0.04988(12) 1.2965(2) 0.98040(13) 0.0684(11) Uiso 0.754(6) 1 d P
HO1 H 0.1875(13) 0.972(2) 0.9486(14) 0.079(9) Uiso 1 1 d .
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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'
P P 0.1023 0.0942 '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'
Ho Ho -0.2175 4.6783 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N3 Fe N3 171.94(8) 2_556 .
N3 Fe N1 82.08(5) 2_556 .
N3 Fe N1 91.98(5) . .
N3 Fe N1 91.98(5) 2_556 2_556
N3 Fe N1 82.08(5) . 2_556
N1 Fe N1 85.57(7) . 2_556
N3 Fe P 92.17(4) 2_556 2_556
N3 Fe P 93.18(4) . 2_556
N1 Fe P 88.96(4) . 2_556
N1 Fe P 172.62(4) 2_556 2_556
N3 Fe P 93.18(4) 2_556 .
N3 Fe P 92.17(4) . .
N1 Fe P 172.62(4) . .
N1 Fe P 88.96(4) 2_556 .
P Fe P 96.90(2) 2_556 .
C12 P C19 104.66(7) . .
C12 P C13 100.34(7) . .
C19 P C13 103.11(7) . .
C12 P Fe 113.17(5) . .
C19 P Fe 120.21(5) . .
C13 P Fe 113.03(5) . .
C6 N3 N2 112.71(13) . .
C6 N3 Fe 135.60(11) . .
N2 N3 Fe 111.59(9) . .
C10 C11 C12 121.85(17) . .
C10 C11 H11 119.1 . .
C12 C11 H11 119.1 . .
C7 C12 C11 118.36(13) . .
C7 C12 P 122.64(11) . .
C11 C12 P 118.92(12) . .
C15 C14 C13 120.07(16) . .
C15 C14 H14 120.0 . .
C13 C14 H14 120.0 . .
C18 C13 C14 118.83(15) . .
C18 C13 P 122.47(12) . .
C14 C13 P 118.54(12) . .
C12 C7 C8 118.79(14) . .
C12 C7 C6 127.26(13) . 2_556
C8 C7 C6 113.83(14) . 2_556
C20 C19 C24 118.30(15) . .
C20 C19 P 122.80(12) . .
C24 C19 P 118.90(12) . .
C11 C10 C9 119.75(16) . .
C11 C10 H10 120.1 . .
C9 C10 H10 120.1 . .
C5 N1 C1 117.75(13) . .
C5 N1 Fe 112.53(10) . .
C1 N1 Fe 129.69(11) . .
C5 N2 N3 118.15(13) 2_556 .
C5 N2 H2 120.9 2_556 .
N3 N2 H2 120.9 . .
C25 O1 HO1 104.6(16) . .
N3 C6 C7 127.84(14) . 2_556
N3 C6 H6 116.1 . .
C7 C6 H6 116.1 2_556 .
C22 C21 C20 120.89(17) . .
C22 C21 H21 119.6 . .
C20 C21 H21 119.6 . .
C9 C8 C7 121.67(17) . .
C9 C8 H8 119.2 . .
C7 C8 H8 119.2 . .
C17 C18 C13 120.37(16) . .
C17 C18 H18 119.8 . .
C13 C18 H18 119.8 . .
C21 C20 C19 120.44(15) . .
C21 C20 H20 119.8 . .
C19 C20 H20 119.8 . .
C17 C16 C15 119.92(17) . .
C17 C16 H16 120.0 . .
C15 C16 H16 120.0 . .
C8 C9 C10 119.53(15) . .
C8 C9 H9 120.2 . .
C10 C9 H9 120.2 . .
C21 C22 C23 119.06(17) . .
C21 C22 H22 120.5 . .
C23 C22 H22 120.5 . .
C23 C24 C19 120.58(16) . .
C23 C24 H24 119.7 . .
C19 C24 H24 119.7 . .
C24 C23 C22 120.66(16) . .
C24 C23 H23 119.7 . .
C22 C23 H23 119.7 . .
C16 C17 C18 120.37(18) . .
C16 C17 H17 119.8 . .
C18 C17 H17 119.8 . .
C16 C15 C14 120.43(16) . .
C16 C15 H15 119.8 . .
C14 C15 H15 119.8 . .
O1 C25 H25A 109.5 . .
O1 C25 H25B 109.5 . .
H25A C25 H25B 109.5 . .
O1 C25 H25C 109.5 . .
H25A C25 H25C 109.5 . .
H25B C25 H25C 109.5 . .
N1 C5 N2 115.43(14) . 2_556
N1 C5 C4 123.09(14) . .
N2 C5 C4 121.47(15) 2_556 .
N1 C1 C2 122.41(15) . .
N1 C1 H1 118.8 . .
C2 C1 H1 118.8 . .
C3 C4 C5 118.03(16) . .
C3 C4 H4 121.0 . .
C5 C4 H4 121.0 . .
C1 C2 C3 119.15(15) . .
C1 C2 H2A 120.4 . .
C3 C2 H2A 120.4 . .
C4 C3 C2 119.50(15) . .
C4 C3 H3 120.3 . .
C2 C3 H3 120.3 . .
O2A C26 O2B 89.4(3) . .
O2A C26 H26A 113.7 . .
O2B C26 H26A 113.7 . .
O2A C26 H26B 113.8 . .
O2B C26 H26B 113.7 . .
H26A C26 H26B 111.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe N3 1.9405(13) 2_556
Fe N3 1.9405(13) .
Fe N1 1.9990(13) .
Fe N1 1.9990(12) 2_556
Fe P 2.2613(4) 2_556
Fe P 2.2613(4) .
P C12 1.8254(15) .
P C19 1.8382(16) .
P C13 1.8413(16) .
N3 C6 1.3062(18) .
N3 N2 1.3824(17) .
C11 C10 1.383(2) .
C11 C12 1.404(2) .
C11 H11 0.9300 .
C12 C7 1.400(2) .
C14 C15 1.390(2) .
C14 C13 1.403(2) .
C14 H14 0.9300 .
C13 C18 1.393(2) .
C7 C8 1.411(2) .
C7 C6 1.451(2) 2_556
C19 C20 1.395(2) .
C19 C24 1.403(2) .
C10 C9 1.383(3) .
C10 H10 0.9300 .
N1 C5 1.347(2) .
N1 C1 1.3540(18) .
N2 C5 1.3564(19) 2_556
N2 H2 0.8600 .
O1 C25 1.409(3) .
O1 HO1 1.00(3) .
C6 C7 1.451(2) 2_556
C6 H6 0.9300 .
C21 C22 1.385(3) .
C21 C20 1.387(2) .
C21 H21 0.9300 .
C8 C9 1.378(2) .
C8 H8 0.9300 .
C18 C17 1.389(2) .
C18 H18 0.9300 .
C20 H20 0.9300 .
C16 C17 1.382(3) .
C16 C15 1.379(3) .
C16 H16 0.9300 .
C9 H9 0.9300 .
C22 C23 1.386(3) .
C22 H22 0.9300 .
C24 C23 1.384(2) .
C24 H24 0.9300 .
C23 H23 0.9300 .
C17 H17 0.9300 .
C15 H15 0.9300 .
C25 H25A 0.9600 .
C25 H25B 0.9600 .
C25 H25C 0.9600 .
C5 N2 1.3564(19) 2_556
C5 C4 1.397(2) .
C1 C2 1.373(2) .
C1 H1 0.9300 .
C4 C3 1.374(2) .
C4 H4 0.9300 .
C2 C3 1.395(2) .
C2 H2A 0.9300 .
C3 H3 0.9300 .
C26 O2A 1.287(5) .
C26 O2B 1.319(3) .
C26 H26A 0.9700 .
C26 H26B 0.9700 .
