#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:53:29 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179768 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/64/7006406.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_7006406
loop_
_publ_author_name
'Elhaïk, Jérôme'
'Kilner, Colin A.'
'Halcrow, Malcolm A.'
_publ_section_title
;
 Structural diversity in iron(II) complexes of
 2,6-di(pyrazol-1-yl)pyridine and 2,6-di(3-methylpyrazol-1-yl)pyridine.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              823
_journal_page_last               830
_journal_paper_doi               10.1039/b510370c
_journal_year                    2006
_chemical_formula_moiety         '[C22 H18 Fe N10], I0.5, [I3]1.5'
_chemical_formula_sum            'C22 H18 Fe I5 N10'
_chemical_formula_weight         1112.81
_chemical_name_systematic
;
Bis[2,6-di(pyrazol-1-yl)pyridine]iron(II) hemiiodide sesqui(triiodide)
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 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                 104.3473(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.9084(3)
_cell_length_b                   13.6094(3)
_cell_length_c                   15.1155(2)
_cell_measurement_reflns_used    41942
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.64
_cell_volume                     3170.50(10)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEX (McArdle, 1995)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
'Nonius KappaCCD area detector diffractometer'
_diffrn_measurement_method       'ω and φ 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  0.1542
_diffrn_reflns_av_sigmaI/netI    0.0768
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            41942
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.64
_exptl_absorpt_coefficient_mu    5.375
_exptl_absorpt_correction_T_max  0.833
_exptl_absorpt_correction_T_min  0.159
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Using multiple and symmetry-related data measurements via the program SORTAV
See R.H. Blessing, Acta Cryst (1995), A51, 33-38
;
_exptl_crystal_colour            Orange-brown
_exptl_crystal_density_diffrn    2.331
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Rectangular prism'
_exptl_crystal_F_000             2044
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.654
_refine_diff_density_min         -2.338
_refine_diff_density_rms         0.302
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         7248
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0489
_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)+(0.0609P)²+1.8604P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1186
_refine_ls_wR_factor_ref         0.1327
_reflns_number_gt                5473
_reflns_number_total             7248
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b510370c.txt
_cod_data_source_block           c:\datasets\leeds\mh139\mh139
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               7006406
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, 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
Fe1 Fe 0.75780(5) 0.85402(5) 0.61215(5) 0.03113(18) Uani 1 1 d . . .
N2 N 0.8128(3) 0.9785(3) 0.5606(3) 0.0299(9) Uani 1 1 d . . .
C3 C 0.8055(3) 1.0680(3) 0.5934(3) 0.0314(11) Uani 1 1 d . . .
C4 C 0.8375(4) 1.1515(4) 0.5616(4) 0.0385(12) Uani 1 1 d . . .
H4 H 0.8312 1.2147 0.5859 0.046 Uiso 1 1 calc R . .
C5 C 0.8793(4) 1.1383(4) 0.4921(4) 0.0425(14) Uani 1 1 d . . .
H5 H 0.9003 1.1941 0.4665 0.051 Uiso 1 1 calc R . .
C6 C 0.8911(3) 1.0461(4) 0.4591(4) 0.0382(12) Uani 1 1 d . . .
H6 H 0.9209 1.0371 0.4125 0.046 Uiso 1 1 calc R . .
C7 C 0.8574(3) 0.9671(4) 0.4974(3) 0.0313(11) Uani 1 1 d . . .
N8 N 0.7604(3) 1.0691(3) 0.6632(3) 0.0326(9) Uani 1 1 d . . .
N9 N 0.7383(3) 0.9801(3) 0.6938(3) 0.0352(10) Uani 1 1 d . . .
C10 C 0.7023(4) 1.0023(4) 0.7618(4) 0.0414(13) Uani 1 1 d . . .
H10 H 0.6802 0.9553 0.7968 0.050 Uiso 1 1 calc R . .
C11 C 0.7011(4) 1.1047(4) 0.7753(4) 0.0454(14) Uani 1 1 d . . .
H11 H 0.6790 1.1389 0.8194 0.054 Uiso 1 1 calc R . .
C12 C 0.7383(4) 1.1440(4) 0.7119(4) 0.0420(13) Uani 1 1 d . . .
H12 H 0.7473 1.2120 0.7031 0.050 Uiso 1 1 calc R . .
N13 N 0.8683(3) 0.8684(3) 0.4766(3) 0.0345(10) Uani 1 1 d . . .
N14 N 0.8416(3) 0.7989(3) 0.5286(3) 0.0364(10) Uani 1 1 d . . .
C15 C 0.8694(4) 0.7133(4) 0.5033(4) 0.0429(13) Uani 1 1 d . . .
H15 H 0.8609 0.6512 0.5285 0.051 Uiso 1 1 calc R . .
C16 C 0.9125(4) 0.7283(5) 0.4348(5) 0.0480(15) Uani 1 1 d . . .
H16 H 0.9374 0.6792 0.4045 0.058 Uiso 1 1 calc R . .
C17 C 0.9122(4) 0.8270(4) 0.4195(4) 0.0416(13) Uani 1 1 d . . .
H17 H 0.9376 0.8602 0.3773 0.050 Uiso 1 1 calc R . .
N18 N 0.6679(3) 0.7341(3) 0.6074(3) 0.0302(9) Uani 1 1 d . . .
C19 C 0.6897(4) 0.6576(4) 0.6635(4) 0.0340(11) Uani 1 1 d . . .
C20 C 0.6376(4) 0.5756(4) 0.6622(4) 0.0403(13) Uani 1 1 d . . .
H20 H 0.6546 0.5227 0.7038 0.048 Uiso 1 1 calc R . .
C21 C 0.5595(4) 0.5754(4) 0.5967(4) 0.0419(13) Uani 1 1 d . . .
H21 H 0.5220 0.5203 0.5925 0.050 Uiso 1 1 calc R . .
C22 C 0.5345(4) 0.6534(4) 0.5371(4) 0.0372(12) Uani 1 1 d . . .
H22 H 0.4811 0.6529 0.4919 0.045 Uiso 1 1 calc R . .
C23 C 0.5902(3) 0.7311(3) 0.5464(3) 0.0308(11) Uani 1 1 d . . .
N24 N 0.7722(3) 0.6692(3) 0.7255(3) 0.0333(9) Uani 1 1 d . . .
N25 N 0.8178(3) 0.7537(3) 0.7213(3) 0.0343(10) Uani 1 1 d . . .
C26 C 0.8908(4) 0.7428(4) 0.7860(4) 0.0394(12) Uani 1 1 d . . .
H26 H 0.9363 0.7898 0.7993 0.047 Uiso 1 1 calc R . .
C27 C 0.8922(4) 0.6534(4) 0.8322(4) 0.0424(13) Uani 1 1 d . . .
H27 H 0.9371 0.6291 0.8810 0.051 Uiso 1 1 calc R . .
C28 C 0.8153(4) 0.6083(4) 0.7923(4) 0.0388(12) Uani 1 1 d . . .
H28 H 0.7960 0.5463 0.8083 0.047 Uiso 1 1 calc R . .
N29 N 0.5733(3) 0.8171(3) 0.4930(3) 0.0332(9) Uani 1 1 d . . .
N30 N 0.6358(3) 0.8888(3) 0.5073(3) 0.0321(9) Uani 1 1 d . . .
C31 C 0.6017(4) 0.9611(4) 0.4512(4) 0.0407(13) Uani 1 1 d . . .
H31 H 0.6297 1.0219 0.4469 0.049 Uiso 1 1 calc R . .
C32 C 0.5180(4) 0.9359(4) 0.3985(4) 0.0425(13) Uani 1 1 d . . .
H32 H 0.4807 0.9743 0.3526 0.051 Uiso 1 1 calc R . .
C33 C 0.5026(4) 0.8451(4) 0.4277(4) 0.0383(12) Uani 1 1 d . . .
H33 H 0.4511 0.8077 0.4061 0.046 Uiso 1 1 calc R . .
I34 I 1.0000 0.99346(4) 0.7500 0.03579(14) Uani 1 2 d S . .
I35 I 0.34381(3) 0.76351(3) 0.60061(3) 0.04655(13) Uani 1 1 d . . .
I36 I 0.5000 0.77632(4) 0.7500 0.03889(15) Uani 1 2 d S . .
I37 I 0.32221(3) 0.62643(3) 0.13843(3) 0.05517(15) Uani 1 1 d . . .
I38 I 0.5000 0.63117(4) 0.2500 0.04252(15) Uani 1 2 d S . .
I39A I 0.1576(8) 0.5628(6) 0.3987(6) 0.073(3) Uani 0.50 1 d PD A 1
I40A I 0.0000 0.5700(8) 0.2500 0.058(4) Uani 0.50 2 d SPD . 1
I39B I 0.1698(17) 0.5648(15) 0.4174(12) 0.069(3) Uani 0.25 1 d PD . 2
I40B I 0.0195(16) 0.5704(6) 0.2592(12) 0.0452(17) Uani 0.25 1 d PD . 2
I41B I -0.1359(9) 0.5717(13) 0.1059(15) 0.066(2) Uani 0.25 1 d PD . 2
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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'
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
N2 Fe1 N18 155.97(16) . . ?
N2 Fe1 N25 129.20(16) . . ?
N18 Fe1 N25 73.31(16) . . ?
N2 Fe1 N9 73.22(16) . . ?
N18 Fe1 N9 115.31(16) . . ?
N25 Fe1 N9 99.32(16) . . ?
N2 Fe1 N14 72.45(16) . . ?
N18 Fe1 N14 102.44(16) . . ?
N25 Fe1 N14 90.41(17) . . ?
N9 Fe1 N14 142.24(17) . . ?
N2 Fe1 N30 86.29(16) . . ?
N18 Fe1 N30 71.62(16) . . ?
N25 Fe1 N30 144.51(16) . . ?
N9 Fe1 N30 90.82(16) . . ?
N14 Fe1 N30 102.14(17) . . ?
C3 N2 C7 119.1(4) . . ?
C3 N2 Fe1 120.5(3) . . ?
C7 N2 Fe1 120.4(3) . . ?
N2 C3 C4 123.4(5) . . ?
N2 C3 N8 113.3(4) . . ?
C4 C3 N8 123.4(5) . . ?
C3 C4 C5 116.4(5) . . ?
C6 C5 C4 121.7(5) . . ?
C5 C6 C7 116.8(5) . . ?
N2 C7 C6 122.4(5) . . ?
N2 C7 N13 113.0(4) . . ?
C6 C7 N13 124.6(5) . . ?
C12 N8 N9 111.0(4) . . ?
C12 N8 C3 131.4(4) . . ?
N9 N8 C3 117.5(4) . . ?
C10 N9 N8 104.9(4) . . ?
C10 N9 Fe1 139.9(4) . . ?
N8 N9 Fe1 114.8(3) . . ?
N9 C10 C11 111.0(5) . . ?
C12 C11 C10 105.4(5) . . ?
N8 C12 C11 107.8(5) . . ?
C17 N13 N14 111.1(4) . . ?
C17 N13 C7 130.6(5) . . ?
N14 N13 C7 117.6(4) . . ?
C15 N14 N13 105.6(5) . . ?
C15 N14 Fe1 139.3(4) . . ?
N13 N14 Fe1 114.6(3) . . ?
N14 C15 C16 110.1(5) . . ?
C17 C16 C15 106.8(5) . . ?
N13 C17 C16 106.4(5) . . ?
C19 N18 C23 117.4(4) . . ?
C19 N18 Fe1 120.3(3) . . ?
C23 N18 Fe1 122.3(3) . . ?
N18 C19 C20 124.0(5) . . ?
N18 C19 N24 112.6(4) . . ?
C20 C19 N24 123.4(5) . . ?
C21 C20 C19 116.1(5) . . ?
C20 C21 C22 121.6(5) . . ?
C23 C22 C21 117.0(5) . . ?
N18 C23 C22 123.8(5) . . ?
N18 C23 N29 112.2(4) . . ?
C22 C23 N29 123.9(5) . . ?
C28 N24 N25 111.9(5) . . ?
C28 N24 C19 129.7(5) . . ?
N25 N24 C19 118.4(4) . . ?
C26 N25 N24 104.4(4) . . ?
C26 N25 Fe1 140.3(4) . . ?
N24 N25 Fe1 115.2(3) . . ?
N25 C26 C27 111.6(5) . . ?
C28 C27 C26 105.5(5) . . ?
N24 C28 C27 106.7(5) . . ?
C33 N29 N30 110.7(4) . . ?
C33 N29 C23 131.0(5) . . ?
N30 N29 C23 118.2(4) . . ?
C31 N30 N29 105.1(4) . . ?
C31 N30 Fe1 139.4(4) . . ?
N29 N30 Fe1 115.4(3) . . ?
N30 C31 C32 111.1(5) . . ?
C33 C32 C31 105.1(5) . . ?
C32 C33 N29 108.0(5) . . ?
I35 I36 I35 173.15(2) . 2_656 ?
I37 I38 I37 177.46(2) 2_655 . ?
I39A I40A I39A 176.2(5) . 2 ?
I39B I40B I41B 177.4(12) . . ?
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 N2 2.141(4) . ?
Fe1 N18 2.159(4) . ?
Fe1 N25 2.171(5) . ?
Fe1 N9 2.181(4) . ?
Fe1 N14 2.185(5) . ?
Fe1 N30 2.231(5) . ?
N2 C3 1.331(6) . ?
N2 C7 1.333(6) . ?
C3 C4 1.380(7) . ?
C3 N8 1.414(7) . ?
C4 C5 1.388(8) . ?
C5 C6 1.379(8) . ?
C6 C7 1.391(7) . ?
C7 N13 1.400(6) . ?
N8 C12 1.354(7) . ?
N8 N9 1.373(6) . ?
N9 C10 1.330(7) . ?
C10 C11 1.409(8) . ?
C11 C12 1.355(9) . ?
N13 C17 1.360(7) . ?
N13 N14 1.362(6) . ?
N14 C15 1.334(7) . ?
C15 C16 1.392(9) . ?
C16 C17 1.363(9) . ?
N18 C19 1.334(7) . ?
N18 C23 1.348(7) . ?
C19 C20 1.386(8) . ?
C19 N24 1.420(7) . ?
C20 C21 1.384(9) . ?
C21 C22 1.386(8) . ?
C22 C23 1.363(7) . ?
C23 N29 1.409(6) . ?
N24 C28 1.354(7) . ?
N24 N25 1.369(6) . ?
N25 C26 1.329(7) . ?
C26 C27 1.402(8) . ?
C27 C28 1.368(8) . ?
N29 C33 1.355(7) . ?
N29 N30 1.372(6) . ?
N30 C31 1.325(7) . ?
C31 C32 1.413(8) . ?
C32 C33 1.355(8) . ?
I35 I36 2.9194(4) . ?
I37 I38 2.9127(5) . ?
I39A I40A 2.925(10) . ?
I39B I40B 2.933(17) . ?
I40B I41B 2.940(16) . ?
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
C4 H4 I39A 0.95 3.04 3.932(10) 157.1 3_676
C4 H4 I39B 0.95 3.00 3.88(2) 154.0 3_676
C4 H4 I41B 0.95 2.96 3.830(19) 153.7 4_675
C6 H6 I34 0.95 3.05 3.999(5) 174.6 3_776
C10 H10 I35 0.95 3.11 4.022(6) 161.9 2_656
C11 H11 I37 0.95 3.26 3.933(6) 129.7 3_676
C15 H15 I39A 0.95 3.15 4.100(11) 175.1 3_666
C15 H15 I39B 0.95 3.12 4.06(2) 171.7 3_666
C15 H15 I41B 0.95 3.25 4.19(2) 169.9 4_665
C16 H16 I40A 0.95 3.13 4.038(8) 160.2 1_655
C16 H16 I40B 0.95 3.18 4.10(2) 161.9 1_655
C17 H17 I34 0.95 3.10 4.033(6) 168.0 3_776
C20 H20 I37 0.95 3.08 4.013(5) 166.1 3_666
C21 H21 I38 0.95 3.23 3.905(6) 129.4 3_666
C26 H26 I34 0.95 3.10 3.926(6) 145.9 .
C28 H28 I37 0.95 3.23 4.150(6) 162.6 3_666
C31 H31 I35 0.95 3.06 3.968(6) 160.3 3_676
