#------------------------------------------------------------------------------
#$Date: 2016-03-25 22:31:57 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180014 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/08/7030829.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_7030829
loop_
_publ_author_name
'Abhervé, Alexandre'
'Clemente-León, Miguel'
'Coronado, Eugenio'
'Gómez-García, Carlos J'
'López-Jordà, Maurici'
_publ_section_title
;
 A spin-crossover complex based on a 2,6-bis(pyrazol-1-yl)pyridine (1-bpp)
 ligand functionalized with a carboxylate group.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9406
_journal_page_last               9409
_journal_paper_doi               10.1039/c4dt00327f
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C24 H18 Cl2 Fe N10 O12'
_chemical_formula_weight         765.23
_chemical_name_common            C2/c
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 105.264(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2679(8)
_cell_length_b                   16.0585(6)
_cell_length_c                   10.7907(5)
_cell_measurement_reflns_used    1956
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.9636
_cell_measurement_theta_min      3.1976
_cell_volume                     2886.7(2)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'SuperNova, Single source at offset), Sapphire3'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0809
_diffrn_reflns_av_unetI/netI     0.0776
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16351
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         3.204
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.793
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93403
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_description       prism
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         3312
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0517
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0340P)²+2.7280P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1171
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2368
_reflns_number_total             3312
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4dt00327f2.cif
_cod_data_source_block           shelx
_cod_depositor_comments          'Adding full bibliography for 7030829.cif.'
_cod_database_code               7030829
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.977
_shelx_estimated_absorpt_t_max   0.984
_shelxl_version_number           2013-4
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
C1 C 0.62320(19) 0.2488(2) 0.0865(3) 0.0257(8) Uani 1 1 d . . .
H1 H 0.6290 0.3075 0.0837 0.031 Uiso 1 1 calc R U .
C2 C 0.66346(19) 0.1908(2) 0.0262(3) 0.0293(8) Uani 1 1 d . . .
H2 H 0.7000 0.2032 -0.0234 0.035 Uiso 1 1 calc R U .
C3 C 0.63914(18) 0.1136(2) 0.0539(3) 0.0240(8) Uani 1 1 d . . .
H3 H 0.6559 0.0615 0.0280 0.029 Uiso 1 1 calc R U .
C4 C 0.54340(17) 0.07072(19) 0.1848(3) 0.0191(7) Uani 1 1 d . . .
C5 C 0.54400(17) -0.01519(19) 0.1787(3) 0.0191(7) Uani 1 1 d . . .
H5 H 0.5730 -0.0440 0.1284 0.023 Uiso 1 1 calc R U .
C6 C 0.5000 -0.0575(3) 0.2500 0.0190(10) Uani 1 2 d S T P
C13 C 0.5000 -0.1507(3) 0.2500 0.0178(10) Uani 1 2 d S T P
C7 C 0.64085(18) 0.2147(2) 0.5016(3) 0.0238(8) Uani 1 1 d . . .
H7 H 0.6488 0.1562 0.5087 0.029 Uiso 1 1 calc R U .
C8 C 0.68403(19) 0.2726(2) 0.5894(3) 0.0275(8) Uani 1 1 d . . .
H8 H 0.7254 0.2610 0.6650 0.033 Uiso 1 1 calc R U .
C9 C 0.65511(18) 0.3488(2) 0.5454(3) 0.0223(7) Uani 1 1 d . . .
H9 H 0.6724 0.4010 0.5843 0.027 Uiso 1 1 calc R U .
C10 C 0.54857(17) 0.39070(18) 0.3474(3) 0.0162(7) Uani 1 1 d . . .
C11 C 0.54863(18) 0.47637(19) 0.3542(3) 0.0183(7) Uani 1 1 d . . .
H11 H 0.5804 0.5052 0.4267 0.022 Uiso 1 1 calc R U .
C12 C 0.5000 0.5187(3) 0.2500 0.0165(9) Uani 1 2 d S T P
C14 C 0.5000 0.6121(3) 0.2500 0.0201(10) Uani 1 2 d S T P
N1 N 0.5000 0.1128(2) 0.2500 0.0171(8) Uani 1 2 d S T P
N3 N 0.57669(14) 0.21013(15) 0.1466(2) 0.0181(6) Uani 1 1 d . . .
N4 N 0.5000 0.3488(2) 0.2500 0.0141(8) Uani 1 2 d S T P
N5 N 0.58739(14) 0.25167(15) 0.4070(2) 0.0183(6) Uani 1 1 d . . .
N7 N 0.58609(15) 0.12593(15) 0.1260(3) 0.0199(6) Uani 1 1 d . . .
N9 N 0.59672(14) 0.33584(15) 0.4353(2) 0.0176(6) Uani 1 1 d . . .
O1 O 0.51950(14) -0.18692(14) 0.1587(2) 0.0297(6) Uani 1 1 d . . .
H1A H 0.5175 -0.2387 0.1682 0.045 Uiso 0.5 1 calc R U P
O1P O 0.77701(16) 0.37281(16) 0.1984(3) 0.0475(7) Uani 1 1 d . . .
O2P O 0.65643(13) 0.44978(14) 0.1517(2) 0.0314(6) Uani 1 1 d . . .
O3 O 0.50968(14) 0.64859(13) 0.3568(2) 0.0311(6) Uani 1 1 d . . .
H3A H 0.5087 0.7004 0.3454 0.047 Uiso 0.5 1 calc R U P
O3P O 0.74490(15) 0.45123(17) 0.3600(2) 0.0427(7) Uani 1 1 d . . .
O4P O 0.78055(14) 0.51818(15) 0.1893(2) 0.0392(7) Uani 1 1 d . . .
Cl1 Cl 0.73947(5) 0.44798(5) 0.22520(8) 0.0246(2) Uani 1 1 d . . .
Fe1 Fe 0.5000 0.23021(4) 0.2500 0.01525(18) Uani 1 2 d S T P
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'
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'
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 C1 C2 110.7(3) . .
C3 C2 C1 106.2(3) . .
N7 C3 C2 106.4(3) . .
N1 C4 C5 122.8(3) . .
N1 C4 N7 110.6(3) . .
C5 C4 N7 126.6(3) . .
C4 C5 C6 116.7(3) . .
C5 C6 C5 121.6(4) . 2_655
C5 C6 C13 119.2(2) . .
C5 C6 C13 119.2(2) 2_655 .
O1 C13 O1 125.1(4) . 2_655
O1 C13 C6 117.4(2) . .
O1 C13 C6 117.4(2) 2_655 .
N5 C7 C8 111.4(3) . .
C9 C8 C7 106.3(3) . .
N9 C9 C8 106.8(3) . .
N4 C10 C11 122.3(3) . .
N4 C10 N9 110.7(3) . .
C11 C10 N9 127.0(3) . .
C10 C11 C12 116.9(3) . .
C11 C12 C11 121.5(4) 2_655 .
C11 C12 C14 119.25(19) 2_655 .
C11 C12 C14 119.25(19) . .
O3 C14 O3 124.8(4) . 2_655
O3 C14 C12 117.6(2) . .
O3 C14 C12 117.6(2) 2_655 .
C4 N1 C4 119.4(4) . 2_655
C4 N1 Fe1 120.31(19) . .
C4 N1 Fe1 120.31(19) 2_655 .
C1 N3 N7 105.6(3) . .
C1 N3 Fe1 142.4(2) . .
N7 N3 Fe1 112.03(19) . .
C10 N4 C10 119.8(3) . 2_655
C10 N4 Fe1 120.12(17) . .
C10 N4 Fe1 120.13(17) 2_655 .
C7 N5 N9 104.5(2) . .
C7 N5 Fe1 143.3(2) . .
N9 N5 Fe1 112.13(17) . .
C3 N7 N3 111.0(3) . .
C3 N7 C4 132.5(3) . .
N3 N7 C4 116.4(3) . .
C9 N9 N5 111.0(2) . .
C9 N9 C10 132.1(3) . .
N5 N9 C10 116.8(2) . .
O3P Cl1 O1P 108.81(17) . .
O3P Cl1 O4P 109.86(16) . .
O1P Cl1 O4P 108.90(17) . .
O3P Cl1 O2P 110.30(16) . .
O1P Cl1 O2P 109.99(15) . .
O4P Cl1 O2P 108.96(14) . .
N1 Fe1 N4 180.0 . .
N1 Fe1 N3 80.58(7) . .
N4 Fe1 N3 99.42(7) . .
N1 Fe1 N3 80.57(7) . 2_655
N4 Fe1 N3 99.43(7) . 2_655
N3 Fe1 N3 161.15(14) . 2_655
N1 Fe1 N5 100.02(7) . .
N4 Fe1 N5 79.98(7) . .
N3 Fe1 N5 92.21(10) . .
N3 Fe1 N5 91.06(10) 2_655 .
N1 Fe1 N5 100.02(7) . 2_655
N4 Fe1 N5 79.98(7) . 2_655
N3 Fe1 N5 91.05(10) . 2_655
N3 Fe1 N5 92.21(10) 2_655 2_655
N5 Fe1 N5 159.95(14) . 2_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N3 1.314(4) .
C1 C2 1.417(5) .
C2 C3 1.368(4) .
C3 N7 1.364(4) .
C4 N1 1.338(3) .
C4 C5 1.381(4) .
C4 N7 1.407(4) .
C5 C6 1.392(4) .
C6 C5 1.392(4) 2_655
C6 C13 1.497(6) .
C13 O1 1.264(3) .
C13 O1 1.264(3) 2_655
C7 N5 1.323(4) .
C7 C8 1.395(5) .
C8 C9 1.359(4) .
C9 N9 1.357(4) .
C10 N4 1.340(3) .
C10 C11 1.378(4) .
C10 N9 1.397(4) .
C11 C12 1.390(3) .
C12 C11 1.390(3) 2_655
C12 C14 1.500(6) .
C14 O3 1.264(3) .
C14 O3 1.264(3) 2_655
N1 C4 1.338(3) 2_655
N1 Fe1 1.886(3) .
N3 N7 1.387(3) .
N3 Fe1 1.970(3) .
N4 C10 1.340(3) 2_655
N4 Fe1 1.904(3) .
N5 N9 1.386(3) .
N5 Fe1 1.980(2) .
O1P Cl1 1.435(3) .
O2P Cl1 1.445(2) .
O3P Cl1 1.433(3) .
O4P Cl1 1.438(2) .
Fe1 N3 1.970(3) 2_655
Fe1 N5 1.980(2) 2_655
