#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:04:44 +0100 (vie 25 de mar de 2016) $
#$Revision: 179878 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/74/7017413.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_7017413
loop_
_publ_author_name
'Kutasi, Anna M.'
'Turner, David R.'
'Moubaraki, Boujemaa'
'Batten, Stuart R.'
'Murray, Keith S.'
_publ_section_title
;
 Complexes of a hexa-nitrile dianion with neutral, chelating co-ligands:
 Self-assembly, structure and magnetism.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12358
_journal_page_last               12367
_journal_paper_doi               10.1039/c1dt11369k
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C22 H15 Fe N9 O2'
_chemical_formula_sum            'C22 H15 Fe N9 O2'
_chemical_formula_weight         493.28
_chemical_name_common            (Fe(pypzH)(HCTMCP)(MeOH)2)
_chemical_name_systematic
;
[Fe(pypzH)(HCTMCP)(MeOH)2]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 98.89(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.9896(16)
_cell_length_b                   15.532(3)
_cell_length_c                   18.130(4)
_cell_measurement_reflns_used    25397
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.68
_cell_volume                     2222.8(8)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Hooft, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'X-Seed (Barbour, 1999)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(1)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_sigmaI/netI    0.0378
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25397
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.68
_exptl_absorpt_coefficient_mu    0.719
_exptl_absorpt_correction_T_max  0.8696
_exptl_absorpt_correction_T_min  0.7719
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SORTAV
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.035
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         5098
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0548
_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)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1127
_refine_ls_wR_factor_ref         0.1191
_reflns_number_gt                4232
_reflns_number_total             5098
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt11369k.txt
_cod_data_source_block           6Fe
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2222.7(8)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7017413
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Fe1 Fe 0.36886(5) 0.33352(2) 0.34802(2) 0.01914(12) Uani 1 1 d .
O1 O 0.1573(2) 0.36808(13) 0.39948(11) 0.0247(4) Uani 1 1 d D
O2 O 0.5858(3) 0.28993(14) 0.30299(11) 0.0279(5) Uani 1 1 d D
N1 N 0.5282(3) 0.34099(15) 0.45484(12) 0.0216(5) Uani 1 1 d .
N2 N 0.5735(4) 0.29148(19) 0.51618(15) 0.0340(6) Uani 1 1 d .
N3 N 0.4795(3) 0.46072(15) 0.34729(12) 0.0213(5) Uani 1 1 d .
N112 N 0.2950(3) 0.20369(15) 0.35560(13) 0.0251(5) Uani 1 1 d .
N114 N -0.0682(5) 0.0592(3) 0.20964(18) 0.0655(11) Uani 1 1 d .
N122 N -0.2254(3) -0.15638(15) 0.26201(13) 0.0238(5) Uani 1 1 d .
N124 N -0.0949(4) -0.26391(18) 0.48562(15) 0.0366(6) Uani 1 1 d .
N132 N 0.4452(4) 0.1191(2) 0.55763(18) 0.0446(8) Uani 1 1 d .
N134 N 0.2820(4) -0.1398(2) 0.63002(17) 0.0472(8) Uani 1 1 d .
C1 C -0.0146(4) 0.3612(3) 0.3616(2) 0.0493(10) Uani 1 1 d .
H1A H -0.0309 0.3050 0.3369 0.074 Uiso 1 1 calc R
H1B H -0.0369 0.4070 0.3242 0.074 Uiso 1 1 calc R
H1C H -0.0929 0.3668 0.3980 0.074 Uiso 1 1 calc R
C2 C 0.6356(5) 0.3097(3) 0.23345(19) 0.0439(9) Uani 1 1 d .
H2A H 0.6548 0.3718 0.2303 0.066 Uiso 1 1 calc R
H2B H 0.5462 0.2921 0.1930 0.066 Uiso 1 1 calc R
H2C H 0.7404 0.2788 0.2288 0.066 Uiso 1 1 calc R
C3 C 0.6962(5) 0.3333(3) 0.56687(17) 0.0439(9) Uani 1 1 d .
H3 H 0.7484 0.3120 0.6140 0.053 Uiso 1 1 calc R
C4 C 0.7278(4) 0.4129(2) 0.53494(16) 0.0294(7) Uani 1 1 d .
H4 H 0.8043 0.4566 0.5554 0.035 Uiso 1 1 calc R
C5 C 0.6211(3) 0.41321(18) 0.46615(15) 0.0209(6) Uani 1 1 d .
C6 C 0.5993(3) 0.47861(17) 0.40672(15) 0.0202(5) Uani 1 1 d .
C7 C 0.6937(4) 0.5535(2) 0.40864(19) 0.0337(7) Uani 1 1 d .
H7 H 0.7763 0.5658 0.4509 0.040 Uiso 1 1 calc R
C8 C 0.6689(5) 0.6086(2) 0.3511(2) 0.0469(9) Uani 1 1 d .
H8 H 0.7338 0.6600 0.3523 0.056 Uiso 1 1 calc R
C9 C 0.5530(5) 0.5908(2) 0.2926(2) 0.0415(8) Uani 1 1 d .
H9 H 0.5358 0.6287 0.2509 0.050 Uiso 1 1 calc R
C10 C 0.4607(4) 0.5191(2) 0.29260(17) 0.0285(6) Uani 1 1 d .
H10 H 0.3756 0.5090 0.2508 0.034 Uiso 1 1 calc R
C101 C 0.1256(3) 0.00016(17) 0.38989(15) 0.0199(5) Uani 1 1 d .
C102 C 0.0650(3) -0.07811(17) 0.41020(14) 0.0193(5) Uani 1 1 d .
C103 C 0.1772(3) -0.03166(17) 0.46118(15) 0.0198(5) Uani 1 1 d .
C110 C 0.1262(4) 0.06423(18) 0.33588(15) 0.0247(6) Uani 1 1 d .
C111 C 0.2207(3) 0.14012(18) 0.34952(15) 0.0216(6) Uani 1 1 d .
C113 C 0.0183(4) 0.0598(2) 0.26628(18) 0.0382(8) Uani 1 1 d .
C120 C -0.0415(3) -0.14935(17) 0.39092(15) 0.0197(5) Uani 1 1 d .
C121 C -0.1428(3) -0.15329(17) 0.32010(15) 0.0196(5) Uani 1 1 d .
C123 C -0.0689(4) -0.21233(18) 0.44406(16) 0.0237(6) Uani 1 1 d .
C130 C 0.2716(3) -0.02055(19) 0.53222(15) 0.0232(6) Uani 1 1 d .
C131 C 0.3696(4) 0.0556(2) 0.54773(17) 0.0295(7) Uani 1 1 d .
C133 C 0.2776(4) -0.0860(2) 0.58625(17) 0.0309(7) Uani 1 1 d .
H1N H 0.525(5) 0.240(3) 0.516(2) 0.052(12) Uiso 1 1 d .
H1O H 0.156(5) 0.336(2) 0.4377(17) 0.060(13) Uiso 1 1 d D
H2O H 0.631(5) 0.2440(18) 0.321(2) 0.056(13) Uiso 1 1 d 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'
N N 0.0061 0.0033 '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'
O O 0.0106 0.0060 '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
N112 Fe1 O1 87.90(9) . .
N112 Fe1 O2 88.48(9) . .
O1 Fe1 O2 175.09(8) . .
N112 Fe1 N122 90.90(9) . 2
O1 Fe1 N122 92.46(9) . 2
O2 Fe1 N122 90.92(9) . 2
N112 Fe1 N1 97.21(9) . .
O1 Fe1 N1 89.51(8) . .
O2 Fe1 N1 87.64(9) . .
N122 Fe1 N1 171.72(9) 2 .
N112 Fe1 N3 171.98(9) . .
O1 Fe1 N3 97.22(8) . .
O2 Fe1 N3 86.03(9) . .
N122 Fe1 N3 95.02(9) 2 .
N1 Fe1 N3 76.75(9) . .
C1 O1 Fe1 122.5(2) . .
C1 O1 H1O 102(3) . .
Fe1 O1 H1O 109(3) . .
C2 O2 Fe1 129.0(2) . .
C2 O2 H2O 111(3) . .
Fe1 O2 H2O 117(3) . .
C5 N1 N2 106.1(2) . .
C5 N1 Fe1 114.76(18) . .
N2 N1 Fe1 139.0(2) . .
N1 N2 C3 110.3(3) . .
N1 N2 H1N 117(3) . .
C3 N2 H1N 133(3) . .
C10 N3 C6 115.8(2) . .
C10 N3 Fe1 128.7(2) . .
C6 N3 Fe1 114.91(18) . .
C111 N112 Fe1 163.8(2) . .
C121 N122 Fe1 176.9(2) . 2_545
O1 C1 H1A 109.5 . .
O1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
O1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
O2 C2 H2A 109.5 . .
O2 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
O2 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
N2 C3 C4 106.9(3) . .
N2 C3 H3 126.5 . .
C4 C3 H3 126.5 . .
C5 C4 C3 104.3(3) . .
C5 C4 H4 127.9 . .
C3 C4 H4 127.9 . .
N1 C5 C4 112.3(3) . .
N1 C5 C6 117.7(2) . .
C4 C5 C6 130.0(3) . .
N3 C6 C7 120.5(3) . .
N3 C6 C5 115.5(2) . .
C7 C6 C5 124.0(3) . .
C8 C7 C6 120.2(3) . .
C8 C7 H7 119.9 . .
C6 C7 H7 119.9 . .
C9 C8 C7 119.4(4) . .
C9 C8 H8 120.3 . .
C7 C8 H8 120.3 . .
C8 C9 C10 119.4(4) . .
C8 C9 H9 120.3 . .
C10 C9 H9 120.3 . .
C9 C10 N3 124.6(3) . .
C9 C10 H10 117.7 . .
N3 C10 H10 117.7 . .
C102 C101 C103 60.19(19) . .
C102 C101 C110 148.7(3) . .
C103 C101 C110 151.1(3) . .
C101 C102 C103 60.12(19) . .
C101 C102 C120 148.3(3) . .
C103 C102 C120 151.5(3) . .
C101 C103 C102 59.69(19) . .
C101 C103 C130 148.8(3) . .
C102 C103 C130 151.5(3) . .
C101 C110 C111 122.4(3) . .
C101 C110 C113 121.5(3) . .
C111 C110 C113 115.8(3) . .
N112 C111 C110 175.3(3) . .
N114 C113 C110 177.7(4) . .
C102 C120 C121 120.0(2) . .
C102 C120 C123 121.8(2) . .
C121 C120 C123 117.6(2) . .
N122 C121 C120 179.8(3) . .
N124 C123 C120 178.1(3) . .
C103 C130 C133 120.5(3) . .
C103 C130 C131 119.1(3) . .
C133 C130 C131 120.3(3) . .
N132 C131 C130 177.0(4) . .
N134 C133 C130 179.5(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N112 2.112(2) .
Fe1 O1 2.122(2) .
Fe1 O2 2.137(2) .
Fe1 N122 2.147(2) 2
Fe1 N1 2.150(2) .
Fe1 N3 2.165(2) .
O1 C1 1.441(4) .
O1 H1O 0.859(19) .
O2 C2 1.413(4) .
O2 H2O 0.839(19) .
N1 C5 1.343(4) .
N1 N2 1.354(3) .
N2 C3 1.396(5) .
N2 H1N 0.89(4) .
N3 C10 1.335(4) .
N3 C6 1.355(3) .
N112 C111 1.149(4) .
N114 C113 1.146(4) .
N122 C121 1.154(4) .
N122 Fe1 2.147(2) 2_545
N124 C123 1.141(4) .
N132 C131 1.156(4) .
N134 C133 1.150(4) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 C4 1.405(5) .
C3 H3 0.9500 .
C4 C5 1.398(4) .
C4 H4 0.9500 .
C5 C6 1.471(4) .
C6 C7 1.383(4) .
C7 C8 1.341(5) .
C7 H7 0.9500 .
C8 C9 1.325(5) .
C8 H8 0.9500 .
C9 C10 1.336(5) .
C9 H9 0.9500 .
C10 H10 0.9500 .
C101 C102 1.380(4) .
C101 C103 1.386(4) .
C101 C110 1.397(4) .
C102 C103 1.387(4) .
C102 C120 1.407(4) .
C103 C130 1.399(4) .
C110 C111 1.401(4) .
C110 C113 1.415(4) .
C120 C121 1.409(4) .
C120 C123 1.413(4) .
C130 C133 1.407(4) .
C130 C131 1.422(4) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H1N N132 0.89(4) 2.15(4) 3.004(4) 160(4) .
O1 H1O N124 0.859(19) 1.90(2) 2.744(3) 166(4) 3_556
O2 H2O N134 0.839(19) 1.93(2) 2.762(4) 173(4) 3_656
