#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:48:41 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179765 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/61/7006108.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_7006108
loop_
_publ_author_name
'Lazar, Hanane Z.'
'Forestier, Thibaut'
'Barrett, Simon A.'
'Kilner, Colin A.'
'Létard, Jean-François'
'Halcrow, Malcolm A.'
_publ_section_title
;
 Thermal and light-induced spin-crossover in salts of the heptadentate
 complex [tris(4-{pyrazol-3-yl}-3-aza-3-butenyl)amine]iron(ii).
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4276
_journal_page_last               4285
_journal_paper_doi               10.1039/b708971f
_journal_year                    2007
_chemical_formula_moiety         'C18 H24 Fe N10, 2[N O3], C H3 N O2'
_chemical_formula_sum            'C19 H27 Fe N13 O8'
_chemical_formula_weight         621.39
_chemical_name_common
;
(Tris-(4-(pyrazol-3-yl)-3-aza-3-butenyl)amine)iron(ii)
dinitrate mono-nitromethane solvate
;
_chemical_name_systematic
;
[Tris-(4-{pyrazol-3-yl}-3-aza-3-butenyl)amine]iron(II)
dinitrate mono-nitromethane solvate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.626(2)
_cell_length_b                   12.574(2)
_cell_length_c                   17.373(3)
_cell_measurement_reflns_used    54613
_cell_measurement_temperature    30(2)
_cell_measurement_theta_max      26.29
_cell_measurement_theta_min      2.00
_cell_volume                     2539.7(7)
_computing_cell_refinement       'APEX 2 software, Bruker Nonius 2004'
_computing_data_collection       'APEX 2 software, Bruker Nonius 2004'
_computing_data_reduction        'SAINT, Bruker Nonius 2004'
_computing_molecular_graphics    'XSEED (Barbour, 2003)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      30(2)
_diffrn_detector_area_resol_mean '120 microns'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker X8 Apex diffractometer'
_diffrn_measurement_method       'Rotation images'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_sigmaI/netI    0.0324
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            54613
_diffrn_reflns_theta_full        26.29
_diffrn_reflns_theta_max         26.29
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.668
_exptl_absorpt_correction_T_max  1.482
_exptl_absorpt_correction_T_min  0.518
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G. M. (2002). SADABS v. 2.03. University of
G/ottingen, Germany.
;
_exptl_crystal_colour            Orange-brown
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Rectangular prism'
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.701
_refine_diff_density_min         -1.114
_refine_diff_density_rms         0.178
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         5096
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.1038
_refine_ls_R_factor_gt           0.0923
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1198P)²+22.5397P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2524
_refine_ls_wR_factor_ref         0.2631
_reflns_number_gt                4559
_reflns_number_total             5096
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b708971f.txt
_cod_data_source_block           mh17230
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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_cell_volume        2539.7(8)
_cod_database_code               7006108
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.41977(10) 0.61307(9) 0.93694(7) 0.0222(3) Uani 1 1 d . . .
N2 N 0.4135(7) 0.8349(7) 0.8238(4) 0.0341(17) Uani 1 1 d . . .
C3 C 0.4794(8) 0.7818(7) 0.7616(5) 0.0254(17) Uani 1 1 d . . .
H3A H 0.5613 0.8025 0.7657 0.030 Uiso 1 1 calc R . .
H3B H 0.4506 0.8069 0.7112 0.030 Uiso 1 1 calc R . .
C4 C 0.4702(10) 0.6600(7) 0.7649(5) 0.036(2) Uani 1 1 d . . .
H4A H 0.3889 0.6389 0.7573 0.043 Uiso 1 1 calc R . .
H4B H 0.5160 0.6289 0.7225 0.043 Uiso 1 1 calc R . .
N5 N 0.5112(6) 0.6174(6) 0.8383(4) 0.0267(15) Uani 1 1 d . . .
C6 C 0.6137(8) 0.5782(6) 0.8411(5) 0.0258(18) Uani 1 1 d . . .
H6 H 0.6626 0.5765 0.7973 0.031 Uiso 1 1 calc R . .
C7 C 0.6501(7) 0.5367(6) 0.9162(5) 0.0225(16) Uani 1 1 d . . .
N8 N 0.5678(6) 0.5431(5) 0.9713(4) 0.0218(14) Uani 1 1 d . . .
N9 N 0.6131(6) 0.4979(5) 1.0341(4) 0.0224(14) Uani 1 1 d . . .
H9 H 0.5770 0.4910 1.0784 0.027 Uiso 1 1 calc R . .
C10 C 0.7243(8) 0.4634(7) 1.0202(5) 0.0267(18) Uani 1 1 d . . .
H10 H 0.7733 0.4287 1.0560 0.032 Uiso 1 1 calc R . .
C11 C 0.7510(8) 0.4881(7) 0.9463(5) 0.0288(18) Uani 1 1 d . . .
H11 H 0.8217 0.4756 0.9204 0.035 Uiso 1 1 calc R . .
C12 C 0.2925(10) 0.8397(8) 0.8232(6) 0.041(2) Uani 1 1 d . . .
H12A H 0.2641 0.8108 0.7738 0.049 Uiso 1 1 calc R . .
H12B H 0.2684 0.9151 0.8263 0.049 Uiso 1 1 calc R . .
C13 C 0.2366(8) 0.7779(7) 0.8896(6) 0.034(2) Uani 1 1 d . . .
H13A H 0.2578 0.8124 0.9388 0.040 Uiso 1 1 calc R . .
H13B H 0.1520 0.7825 0.8842 0.040 Uiso 1 1 calc R . .
N14 N 0.2697(7) 0.6663(6) 0.8929(4) 0.0307(17) Uani 1 1 d . . .
C15 C 0.1994(8) 0.5947(8) 0.8663(5) 0.034(2) Uani 1 1 d . . .
H15 H 0.1269 0.6127 0.8446 0.040 Uiso 1 1 calc R . .
C16 C 0.2396(8) 0.4840(7) 0.8722(5) 0.0281(19) Uani 1 1 d . . .
N17 N 0.3479(6) 0.4749(6) 0.9050(4) 0.0230(14) Uani 1 1 d . . .
N18 N 0.3718(7) 0.3694(5) 0.9047(4) 0.0247(14) Uani 1 1 d . . .
H18 H 0.4358 0.3411 0.9224 0.030 Uiso 1 1 calc R . .
C19 C 0.2832(8) 0.3130(7) 0.8730(5) 0.0290(19) Uani 1 1 d . . .
H19 H 0.2813 0.2380 0.8666 0.035 Uiso 1 1 calc R . .
C20 C 0.1970(10) 0.3824(9) 0.8519(5) 0.038(2) Uani 1 1 d . . .
H20 H 0.1250 0.3657 0.8289 0.046 Uiso 1 1 calc R . .
C21 C 0.4758(9) 0.8980(8) 0.8790(6) 0.037(2) Uani 1 1 d . . .
H21A H 0.4204 0.9431 0.9074 0.044 Uiso 1 1 calc R . .
H21B H 0.5289 0.9458 0.8510 0.044 Uiso 1 1 calc R . .
C22 C 0.5461(9) 0.8320(8) 0.9380(6) 0.037(2) Uani 1 1 d . . .
H22A H 0.6078 0.7927 0.9108 0.044 Uiso 1 1 calc R . .
H22B H 0.5828 0.8804 0.9756 0.044 Uiso 1 1 calc R . .
N23 N 0.4711(6) 0.7558(6) 0.9790(4) 0.0258(15) Uani 1 1 d . . .
C24 C 0.4392(7) 0.7795(6) 1.0470(5) 0.0251(18) Uani 1 1 d . . .
H24 H 0.4587 0.8452 1.0706 0.030 Uiso 1 1 calc R . .
C25 C 0.3699(8) 0.6979(6) 1.0866(4) 0.0219(16) Uani 1 1 d . . .
N26 N 0.3514(6) 0.6107(6) 1.0436(3) 0.0217(13) Uani 1 1 d . . .
N27 N 0.2949(6) 0.5432(5) 1.0907(4) 0.0210(14) Uani 1 1 d . . .
H27 H 0.2709 0.4794 1.0772 0.025 Uiso 1 1 calc R . .
C28 C 0.2800(7) 0.5861(6) 1.1608(5) 0.0221(16) Uani 1 1 d . . .
H28 H 0.2449 0.5514 1.2033 0.027 Uiso 1 1 calc R . .
C29 C 0.3228(7) 0.6866(6) 1.1618(5) 0.0222(16) Uani 1 1 d . . .
H29 H 0.3217 0.7369 1.2026 0.027 Uiso 1 1 calc R . .
N30 N 0.5673(7) 0.1786(7) 0.9500(4) 0.0356(18) Uani 1 1 d . . .
O31 O 0.5882(7) 0.2738(5) 0.9429(4) 0.0405(16) Uani 1 1 d . . .
O32 O 0.4684(8) 0.1474(7) 0.9359(6) 0.059(2) Uani 1 1 d . . .
O33 O 0.6429(8) 0.1135(9) 0.9681(4) 0.064(3) Uani 1 1 d . . .
N34 N 0.5930(6) 0.4435(5) 1.2293(4) 0.0232(15) Uani 1 1 d . . .
O35 O 0.5180(6) 0.4861(5) 1.1830(3) 0.0283(13) Uani 1 1 d . . .
O36 O 0.5758(6) 0.4459(5) 1.2993(3) 0.0330(14) Uani 1 1 d . . .
O37 O 0.6808(5) 0.4027(5) 1.2015(3) 0.0298(14) Uani 1 1 d . . .
C38 C 0.4048(11) 0.2623(10) 1.0918(6) 0.048(3) Uani 1 1 d . . .
H38A H 0.4683 0.3078 1.0747 0.072 Uiso 1 1 calc R . .
H38B H 0.3365 0.2770 1.0605 0.072 Uiso 1 1 calc R . .
H38C H 0.4267 0.1875 1.0859 0.072 Uiso 1 1 calc R . .
N39 N 0.3791(7) 0.2845(7) 1.1734(5) 0.0367(19) Uani 1 1 d . . .
O40 O 0.4418(7) 0.2455(6) 1.2243(4) 0.0441(18) Uani 1 1 d . . .
O41 O 0.2935(7) 0.3401(6) 1.1880(4) 0.0431(17) Uani 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'
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'
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
N17 Fe1 N26 94.4(3) . . ?
N17 Fe1 N5 90.4(3) . . ?
N26 Fe1 N5 171.4(3) . . ?
N17 Fe1 N14 79.7(3) . . ?
N26 Fe1 N14 90.7(3) . . ?
N5 Fe1 N14 97.1(3) . . ?
N17 Fe1 N8 93.4(3) . . ?
N26 Fe1 N8 93.3(3) . . ?
N5 Fe1 N8 79.3(3) . . ?
N14 Fe1 N8 172.3(3) . . ?
N17 Fe1 N23 171.4(3) . . ?
N26 Fe1 N23 78.3(3) . . ?
N5 Fe1 N23 97.3(3) . . ?
N14 Fe1 N23 95.6(3) . . ?
N8 Fe1 N23 91.6(3) . . ?
N17 Fe1 N2 122.6(2) . . ?
N26 Fe1 N2 122.2(2) . . ?
N5 Fe1 N2 60.0(2) . . ?
N14 Fe1 N2 59.5(3) . . ?
N8 Fe1 N2 122.9(2) . . ?
N23 Fe1 N2 59.4(2) . . ?
C12 N2 C21 118.9(8) . . ?
C12 N2 C3 122.1(8) . . ?
C21 N2 C3 118.3(8) . . ?
C12 N2 Fe1 93.4(6) . . ?
C21 N2 Fe1 93.2(5) . . ?
C3 N2 Fe1 92.3(5) . . ?
N2 C3 C4 112.7(8) . . ?
N5 C4 C3 112.0(8) . . ?
C6 N5 C4 118.3(8) . . ?
C6 N5 Fe1 116.3(6) . . ?
C4 N5 Fe1 125.4(6) . . ?
N5 C6 C7 115.9(7) . . ?
N8 C7 C11 110.3(7) . . ?
N8 C7 C6 113.7(7) . . ?
C11 C7 C6 135.9(8) . . ?
N9 N8 C7 105.9(7) . . ?
N9 N8 Fe1 139.4(6) . . ?
C7 N8 Fe1 114.7(6) . . ?
N8 N9 C10 110.9(7) . . ?
C11 C10 N9 107.9(8) . . ?
C10 C11 C7 104.9(8) . . ?
N2 C12 C13 113.4(8) . . ?
N14 C13 C12 113.9(8) . . ?
C15 N14 C13 119.1(9) . . ?
C15 N14 Fe1 116.7(6) . . ?
C13 N14 Fe1 124.2(7) . . ?
N14 C15 C16 115.4(8) . . ?
N17 C16 C20 110.2(8) . . ?
N17 C16 C15 113.3(8) . . ?
C20 C16 C15 136.5(9) . . ?
N18 N17 C16 105.4(7) . . ?
N18 N17 Fe1 139.7(6) . . ?
C16 N17 Fe1 114.9(6) . . ?
N17 N18 C19 110.8(7) . . ?
N18 C19 C20 109.1(8) . . ?
C19 C20 C16 104.5(9) . . ?
N2 C21 C22 114.2(8) . . ?
N23 C22 C21 110.7(8) . . ?
C24 N23 C22 117.9(8) . . ?
C24 N23 Fe1 117.1(6) . . ?
C22 N23 Fe1 124.9(6) . . ?
N23 C24 C25 115.4(7) . . ?
N26 C25 C29 111.6(7) . . ?
N26 C25 C24 113.4(7) . . ?
C29 C25 C24 135.0(7) . . ?
C25 N26 N27 104.7(6) . . ?
C25 N26 Fe1 115.8(6) . . ?
N27 N26 Fe1 139.3(6) . . ?
C28 N27 N26 111.1(6) . . ?
N27 C28 C29 109.8(7) . . ?
C28 C29 C25 102.8(7) . . ?
O31 N30 O32 118.2(9) . . ?
O31 N30 O33 121.9(10) . . ?
O32 N30 O33 119.8(10) . . ?
O36 N34 O37 121.8(7) . . ?
O36 N34 O35 119.3(7) . . ?
O37 N34 O35 118.8(7) . . ?
O41 N39 O40 123.1(9) . . ?
O41 N39 C38 117.6(8) . . ?
O40 N39 C38 119.2(9) . . ?
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 N17 2.006(8) . ?
Fe1 N26 2.016(6) . ?
Fe1 N5 2.018(7) . ?
Fe1 N14 2.019(9) . ?
Fe1 N8 2.023(8) . ?
Fe1 N23 2.028(8) . ?
Fe1 N2 3.414(8) . ?
N2 C12 1.408(14) . ?
N2 C21 1.440(14) . ?
N2 C3 1.483(11) . ?
C3 C4 1.537(11) . ?
C4 N5 1.462(12) . ?
N5 C6 1.291(12) . ?
C6 C7 1.467(12) . ?
C7 N8 1.356(11) . ?
C7 C11 1.423(13) . ?
N8 N9 1.338(10) . ?
N9 C10 1.386(12) . ?
C10 C11 1.356(13) . ?
C12 C13 1.534(14) . ?
C13 N14 1.457(11) . ?
N14 C15 1.300(13) . ?
C15 C16 1.472(13) . ?
C16 N17 1.387(12) . ?
C16 C20 1.415(14) . ?
N17 N18 1.356(10) . ?
N18 C19 1.366(12) . ?
C19 C20 1.379(15) . ?
C21 C22 1.552(14) . ?
C22 N23 1.478(12) . ?
N23 C24 1.273(11) . ?
C24 C25 1.475(12) . ?
C25 N26 1.344(11) . ?
C25 C29 1.424(11) . ?
N26 N27 1.350(10) . ?
N27 C28 1.344(11) . ?
C28 C29 1.359(12) . ?
N30 O31 1.227(11) . ?
N30 O32 1.239(12) . ?
N30 O33 1.242(11) . ?
N34 O36 1.234(9) . ?
N34 O37 1.239(9) . ?
N34 O35 1.301(9) . ?
C38 N39 1.477(14) . ?
N39 O41 1.242(11) . ?
N39 O40 1.247(11) . ?
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
N9 H9 O35 0.88 1.94 2.817(9) 171.2 .
C10 H10 O32 0.95 2.47 3.252(13) 140.0 3_557
N18 H18 O31 0.88 2.00 2.866(11) 169.7 .
C19 H19 O37 0.95 2.43 3.233(10) 142.4 3_457
N27 H27 O33 0.88 2.05 2.836(10) 148.3 3_457
