#------------------------------------------------------------------------------
#$Date: 2017-01-03 18:24:05 +0200 (Tue, 03 Jan 2017) $
#$Revision: 189766 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/54/4315424.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_4315424
loop_
_publ_author_name
'Vadapalli Chandrasekhar'
'Ramachandran Azhakar'
'Balasubramanian Murugesapandian'
'Tapas Senapati'
'Prasenjit Bag'
'Mrituanjay D. Pandey'
'Sandeep Kumar Maurya'
'Debabrata Goswami'
_publ_contact_author_address
;Head, Department of Chemistry
Indian Institute of Technology Kanpur
Kanpur 208016
Uttarpradesh
India
;
_publ_contact_author_email       vc@iitk.ac.in
_publ_contact_author_fax         '+91-512-259 7436'
_publ_contact_author_name        'Prof. V. Chandrasekhar'
_publ_contact_author_phone       '+91-512-259 7259'
_publ_section_title
;
 Synthesis, Structure, and Two-Photon Absorption Studies of a
 Phosphorus-Based Tris Hydrazone Ligand
 (S)P[N(Me)N=CH-C6H3-2-OH-4-N(CH2CH3)2]3 and Its Metal Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4008
_journal_page_last               4016
_journal_paper_doi               10.1021/ic901531e
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C36 H55 Fe N9 O5 P S'
_chemical_formula_weight         812.77
_chemical_name_systematic        ?
_space_group_IT_number           165
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 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                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                120.000(5)
_cell_formula_units_Z            4
_cell_length_a                   12.073(5)
_cell_length_b                   12.073(5)
_cell_length_c                   32.033(5)
_cell_measurement_temperature    100(2)
_cell_volume                     4044(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.935
_diffrn_measured_fraction_theta_max 0.935
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0944
_diffrn_reflns_av_sigmaI/netI    0.0798
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            11230
_diffrn_reflns_theta_full        22.49
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    0.516
_exptl_absorpt_correction_T_max  0.9599
_exptl_absorpt_correction_T_min  0.9406
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1724
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.118
_refine_diff_density_min         -1.732
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         1655
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.1881
_refine_ls_R_factor_gt           0.1766
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0935P)²+158.2839P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4215
_refine_ls_wR_factor_ref         0.4259
_reflns_number_gt                1389
_reflns_number_total             1655
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901531e_si_002_1.cif
_cod_data_source_block           Complex-2
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2017-01-03

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4315424
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Fe1 Fe 0.6667 0.3333 0.29469(11) 0.0253(12) Uani 1 3 d S . . 0
P1 P 0.6667 0.3333 0.1885(2) 0.0301(18) Uani 1 3 d S . . 0
S1 S 0.6667 0.3333 0.1283(2) 0.0345(19) Uani 1 3 d S . . 0
N1 N 0.6940(12) 0.4699(13) 0.2093(3) 0.028(3) Uani 1 1 d . . . 0
N2 N 0.7408(13) 0.4916(13) 0.2528(4) 0.035(3) Uani 1 1 d . . . 0
N3 N 1.1017(16) 0.8006(15) 0.4095(4) 0.051(4) Uani 1 1 d . . . 0
O1 O 0.8165(11) 0.4448(11) 0.3276(3) 0.039(3) Uani 1 1 d . . . 0
O2 O 0.6667 0.3333 0.417(2) 0.20(2) Uiso 1 3 d S . . 2
O3 O 0.0000 0.0000 0.3056(16) 0.159(18) Uiso 1 3 d S . . 2
C1 C 0.6170(18) 0.5250(18) 0.2000(5) 0.042(4) Uani 1 1 d . . . 0
H1A H 0.5386 0.4830 0.2167 0.064 Uiso 1 1 calc R . . 0
H1B H 0.5950 0.5136 0.1703 0.064 Uiso 1 1 calc R . . 0
H1C H 0.6644 0.6165 0.2066 0.064 Uiso 1 1 calc R . . 0
C2 C 0.8178(15) 0.6071(15) 0.2623(4) 0.031(4) Uani 1 1 d . . . 0
H2 H 0.8347 0.6694 0.2414 0.037 Uiso 1 1 calc R . . 0
C3 C 0.8816(16) 0.6525(16) 0.3013(4) 0.030(4) Uani 1 1 d . . . 0
C4 C 0.8817(14) 0.5671(14) 0.3314(5) 0.028(4) Uani 1 1 d . . . 0
C5 C 0.9574(15) 0.6196(16) 0.3681(4) 0.030(4) Uani 1 1 d . . . 0
H5 H 0.9597 0.5639 0.3886 0.036 Uiso 1 1 calc R . . 0
C6 C 1.0290(17) 0.7533(19) 0.3743(5) 0.042(5) Uani 1 1 d . . . 0
C7 C 1.0274(15) 0.8346(16) 0.3435(5) 0.032(4) Uani 1 1 d . . . 0
H7 H 1.0760 0.9248 0.3470 0.038 Uiso 1 1 calc R . . 0
C8 C 0.9564(14) 0.7839(14) 0.3089(5) 0.031(4) Uani 1 1 d . . . 0
H8 H 0.9572 0.8410 0.2884 0.037 Uiso 1 1 calc R . . 0
C9 C 1.115(2) 0.718(2) 0.4412(7) 0.062(6) Uani 1 1 d . . . 0
H9A H 1.1145 0.6448 0.4270 0.075 Uiso 1 1 calc R . . 0
H9B H 1.1979 0.7675 0.4557 0.075 Uiso 1 1 calc R . . 0
C10 C 1.011(3) 0.668(2) 0.4723(6) 0.071(7) Uani 1 1 d . . . 0
H10A H 1.0102 0.7404 0.4864 0.106 Uiso 1 1 calc R . . 0
H10B H 1.0242 0.6165 0.4930 0.106 Uiso 1 1 calc R . . 0
H10C H 0.9285 0.6158 0.4583 0.106 Uiso 1 1 calc R . . 0
C11 C 1.165(2) 0.937(2) 0.4201(6) 0.069(7) Uani 1 1 d . . . 0
H11A H 1.1654 0.9474 0.4507 0.083 Uiso 1 1 calc R . . 0
H11B H 1.1161 0.9753 0.4077 0.083 Uiso 1 1 calc R . . 0
C12 C 1.304(2) 1.008(2) 0.4034(7) 0.069(6) Uani 1 1 d . . . 0
H12A H 1.3523 0.9722 0.4161 0.103 Uiso 1 1 calc R . . 0
H12B H 1.3438 1.0995 0.4105 0.103 Uiso 1 1 calc R . . 0
H12C H 1.3029 0.9988 0.3730 0.103 Uiso 1 1 calc R . . 0
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'
O O 0.0106 0.0060 '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'
S S 0.1246 0.1234 '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'
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
_geom_angle_publ_flag
O1 Fe1 O1 93.2(5) 2_655 . ?
O1 Fe1 O1 93.2(5) 2_655 3_665 ?
O1 Fe1 O1 93.2(5) . 3_665 ?
O1 Fe1 N2 83.8(5) 2_655 2_655 ?
O1 Fe1 N2 167.4(5) . 2_655 ?
O1 Fe1 N2 99.1(5) 3_665 2_655 ?
O1 Fe1 N2 99.1(5) 2_655 . ?
O1 Fe1 N2 83.8(5) . . ?
O1 Fe1 N2 167.4(5) 3_665 . ?
N2 Fe1 N2 84.6(5) 2_655 . ?
O1 Fe1 N2 167.4(5) 2_655 3_665 ?
O1 Fe1 N2 99.1(5) . 3_665 ?
O1 Fe1 N2 83.8(5) 3_665 3_665 ?
N2 Fe1 N2 84.6(5) 2_655 3_665 ?
N2 Fe1 N2 84.6(5) . 3_665 ?
N1 P1 N1 104.9(5) 3_665 2_655 ?
N1 P1 N1 104.9(5) 3_665 . ?
N1 P1 N1 104.9(5) 2_655 . ?
N1 P1 S1 113.7(4) 3_665 . ?
N1 P1 S1 113.7(4) 2_655 . ?
N1 P1 S1 113.7(4) . . ?
C1 N1 N2 113.3(12) . . ?
C1 N1 P1 122.2(11) . . ?
N2 N1 P1 115.1(10) . . ?
C2 N2 N1 115.2(13) . . ?
C2 N2 Fe1 125.8(11) . . ?
N1 N2 Fe1 118.9(10) . . ?
C6 N3 C11 121.5(16) . . ?
C6 N3 C9 123.0(16) . . ?
C11 N3 C9 115.3(15) . . ?
C4 O1 Fe1 132.1(10) . . ?
N2 C2 C3 126.3(15) . . ?
C8 C3 C4 118.2(14) . . ?
C8 C3 C2 120.5(14) . . ?
C4 C3 C2 121.0(15) . . ?
O1 C4 C3 123.4(14) . . ?
O1 C4 C5 118.4(14) . . ?
C3 C4 C5 118.1(14) . . ?
C6 C5 C4 120.9(15) . . ?
N3 C6 C7 121.3(17) . . ?
N3 C6 C5 119.5(16) . . ?
C7 C6 C5 119.2(14) . . ?
C8 C7 C6 119.4(16) . . ?
C7 C8 C3 124.2(15) . . ?
C10 C9 N3 112.1(18) . . ?
N3 C11 C12 111(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O1 1.940(11) 2_655 ?
Fe1 O1 1.940(11) . ?
Fe1 O1 1.940(11) 3_665 ?
Fe1 N2 2.131(13) 2_655 ?
Fe1 N2 2.131(13) . ?
Fe1 N2 2.132(13) 3_665 ?
P1 N1 1.651(14) 3_665 ?
P1 N1 1.651(14) 2_655 ?
P1 N1 1.651(14) . ?
P1 S1 1.930(9) . ?
N1 C1 1.42(2) . ?
N1 N2 1.479(18) . ?
N2 C2 1.27(2) . ?
N3 C6 1.37(2) . ?
N3 C11 1.47(3) . ?
N3 C9 1.49(2) . ?
O1 C4 1.285(18) . ?
C2 C3 1.43(2) . ?
C3 C8 1.40(2) . ?
C3 C4 1.41(2) . ?
C4 C5 1.43(2) . ?
C5 C6 1.41(3) . ?
C6 C7 1.40(2) . ?
C7 C8 1.35(2) . ?
C9 C10 1.48(3) . ?
C11 C12 1.55(3) . ?
