#------------------------------------------------------------------------------
#$Date: 2019-11-17 13:38:49 +0200 (Sun, 17 Nov 2019) $
#$Revision: 230212 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/78/7057809.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_7057809
loop_
_publ_author_name
'Mason, Helen E.'
'Hamilton, Michelle L.'
'Howard, Judith A. K.'
'Sparkes, Hazel A.'
_publ_section_title
;
 [Fe(abpt)2(NCSe)2] polymorph A: structural studies into the spin
 crossover behaviour
;
_journal_issue                   22
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18028
_journal_paper_doi               10.1039/C8NJ03627F
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C26 H20 Fe N14 Se2'
_chemical_formula_sum            'C26 H20 Fe N14 Se2'
_chemical_formula_weight         742.33
_chemical_name_common            '[Fe(abpt)2(NCSe)2] polymorph A'
_chemical_name_systematic
bis(4-amino-3,5-bis(pyridin-2-yl)-1,2,4-triazole)-bis(isoselenocyanato)-iron(II)
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-08-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-08-14 deposited with the CCDC.
2018-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.1650(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.4971(3)
_cell_length_b                   10.0240(4)
_cell_length_c                   16.4110(6)
_cell_measurement_reflns_used    9267
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.264
_cell_measurement_theta_min      2.382
_cell_volume                     1395.67(9)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'SMART v5.049 (Bruker, 1999)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker SMART CCD 1K area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 1K area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15588
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_min         2.382
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.195
_exptl_absorpt_correction_T_max  0.6255
_exptl_absorpt_correction_T_min  0.4988
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction (numerical with multi-scan). wR2(int) was 0.0781 before and 0.0531 after correction. The Ratio of minimum to maximum transmission is 0.7974. The λ/2 correction factor is 0.0015.'
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_description       block
_exptl_crystal_F_000             736
_exptl_crystal_preparation
'Slow diffusion of abpt ligand in methanol solution into 1:1 methanol:water Fe2+/2(NCSe-) solution'
_exptl_crystal_recrystallization_method 'water/methanol slow diffusion'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.639
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         2861
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0295
_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)+(0.0195P)²+1.5952P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0633
_refine_ls_wR_factor_ref         0.0649
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2575
_reflns_number_total             2861
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8nj03627f2.cif
_cod_data_source_block           200K
_cod_depositor_comments
'Adding full bibliography for 7057796--7057812.cif.'
_cod_database_code               7057809
_shelx_shelxl_version_number     2017/1
_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_max   0.629
_shelx_estimated_absorpt_t_min   0.490
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12), C13(H13)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Se1 Se 0.26255(3) 0.72438(3) 0.25731(2) 0.03822(10) Uani 1 1 d . . .
Fe1 Fe 0.500000 0.500000 0.500000 0.02069(12) Uani 1 2 d S T P
N1 N 0.4008(2) 0.5711(2) 0.39751(13) 0.0272(5) Uani 1 1 d . . .
N2 N 0.7083(2) 0.5852(2) 0.47385(12) 0.0273(5) Uani 1 1 d . . .
N3 N 0.4763(2) 0.6789(2) 0.54814(12) 0.0270(4) Uani 1 1 d . . .
N4 N 0.3572(2) 0.7490(2) 0.58046(13) 0.0263(5) Uani 1 1 d . . .
N5 N 0.5669(2) 0.8772(2) 0.57833(13) 0.0276(5) Uani 1 1 d . . .
N6 N 0.6764(3) 0.9844(2) 0.59056(15) 0.0339(5) Uani 1 1 d . . .
H6A H 0.735(4) 0.965(3) 0.6436(19) 0.041 Uiso 1 1 d R . .
H6B H 0.617(4) 1.056(3) 0.6016(18) 0.041 Uiso 1 1 d R . .
N7 N 0.3904(2) 1.0926(2) 0.64531(13) 0.0307(5) Uani 1 1 d . . .
C1 C 0.3449(3) 0.6291(2) 0.34236(16) 0.0261(5) Uani 1 1 d . . .
C2 C 0.8190(3) 0.5310(3) 0.42861(16) 0.0323(6) Uani 1 1 d . . .
H2 H 0.798578 0.446845 0.403598 0.039 Uiso 1 1 calc R . .
C3 C 0.9618(3) 0.5933(3) 0.41708(18) 0.0368(6) Uani 1 1 d . . .
H3 H 1.036575 0.553056 0.383837 0.044 Uiso 1 1 calc R . .
C4 C 0.9942(3) 0.7140(3) 0.45421(18) 0.0397(7) Uani 1 1 d . . .
H4 H 1.092861 0.756489 0.448339 0.048 Uiso 1 1 calc R . .
C5 C 0.8809(3) 0.7731(3) 0.50048(17) 0.0351(6) Uani 1 1 d . . .
H5 H 0.900169 0.856597 0.526558 0.042 Uiso 1 1 calc R . .
C6 C 0.7393(3) 0.7069(3) 0.50744(15) 0.0271(5) Uani 1 1 d . . .
C7 C 0.6019(3) 0.7568(2) 0.54629(15) 0.0265(5) Uani 1 1 d . . .
C8 C 0.4134(3) 0.8680(2) 0.59901(15) 0.0260(5) Uani 1 1 d . . .
C9 C 0.3228(3) 0.9727(2) 0.63836(15) 0.0276(5) Uani 1 1 d . . .
C10 C 0.3123(3) 1.1860(3) 0.68501(17) 0.0348(6) Uani 1 1 d . . .
H10 H 0.359491 1.271445 0.692070 0.042 Uiso 1 1 calc R . .
C11 C 0.1667(3) 1.1649(3) 0.71632(16) 0.0324(6) Uani 1 1 d . . .
H11 H 0.116045 1.234171 0.744423 0.039 Uiso 1 1 calc R . .
C12 C 0.0960(3) 1.0418(3) 0.70618(17) 0.0336(6) Uani 1 1 d . . .
H12 H -0.005221 1.025326 0.725882 0.040 Uiso 1 1 calc R . .
C13 C 0.1763(3) 0.9421(3) 0.66641(16) 0.0314(6) Uani 1 1 d . . .
H13 H 0.131936 0.855720 0.658746 0.038 Uiso 1 1 calc R . .
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 1.00 0.00 0.105
0.00 -1.00 0.00 0.105
1.00 0.00 1.00 0.130
-1.00 0.00 1.00 0.130
0.00 0.00 -1.00 0.080
0.00 0.00 1.00 0.080
-1.00 0.00 -1.00 0.130
1.00 0.00 -1.00 0.130
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
N1 Fe1 N1 180.0 . 3_666
N1 Fe1 N2 90.24(8) 3_666 3_666
N1 Fe1 N2 89.76(8) 3_666 .
N1 Fe1 N2 89.76(8) . 3_666
N1 Fe1 N2 90.24(8) . .
N1 Fe1 N3 87.98(8) . .
N1 Fe1 N3 87.98(8) 3_666 3_666
N1 Fe1 N3 92.02(8) 3_666 .
N1 Fe1 N3 92.02(8) . 3_666
N2 Fe1 N2 180.0 . 3_666
N3 Fe1 N2 100.83(8) 3_666 .
N3 Fe1 N2 79.17(8) . .
N3 Fe1 N2 79.17(8) 3_666 3_666
N3 Fe1 N2 100.83(8) . 3_666
N3 Fe1 N3 180.0 . 3_666
C1 N1 Fe1 170.9(2) . .
C2 N2 Fe1 126.19(18) . .
C2 N2 C6 117.5(2) . .
C6 N2 Fe1 116.32(16) . .
N4 N3 Fe1 135.93(16) . .
C7 N3 Fe1 115.19(16) . .
C7 N3 N4 108.8(2) . .
C8 N4 N3 106.9(2) . .
C7 N5 N6 124.6(2) . .
C7 N5 C8 105.6(2) . .
C8 N5 N6 129.6(2) . .
N5 N6 H6A 105.3(17) . .
N5 N6 H6B 105.0(19) . .
H6A N6 H6B 104(3) . .
C9 N7 C10 116.7(2) . .
N1 C1 Se1 178.0(2) . .
N2 C2 H2 118.8 . .
N2 C2 C3 122.5(3) . .
C3 C2 H2 118.8 . .
C2 C3 H3 120.3 . .
C4 C3 C2 119.4(3) . .
C4 C3 H3 120.3 . .
C3 C4 H4 120.4 . .
C3 C4 C5 119.3(3) . .
C5 C4 H4 120.4 . .
C4 C5 H5 120.9 . .
C6 C5 C4 118.1(3) . .
C6 C5 H5 120.9 . .
N2 C6 C5 123.2(2) . .
N2 C6 C7 110.2(2) . .
C5 C6 C7 126.5(2) . .
N3 C7 N5 108.7(2) . .
N3 C7 C6 118.5(2) . .
N5 C7 C6 132.6(2) . .
N4 C8 N5 110.0(2) . .
N4 C8 C9 123.8(2) . .
N5 C8 C9 126.1(2) . .
N7 C9 C8 116.5(2) . .
N7 C9 C13 124.2(2) . .
C13 C9 C8 119.3(2) . .
N7 C10 H10 118.3 . .
N7 C10 C11 123.5(3) . .
C11 C10 H10 118.3 . .
C10 C11 H11 120.5 . .
C12 C11 C10 119.0(2) . .
C12 C11 H11 120.5 . .
C11 C12 H12 120.7 . .
C11 C12 C13 118.5(2) . .
C13 C12 H12 120.7 . .
C9 C13 C12 118.0(2) . .
C9 C13 H13 121.0 . .
C12 C13 H13 121.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Se1 C1 1.800(3) .
Fe1 N1 1.973(2) 3_666
Fe1 N1 1.973(2) .
Fe1 N2 2.032(2) .
Fe1 N2 2.032(2) 3_666
Fe1 N3 1.974(2) 3_666
Fe1 N3 1.974(2) .
N1 C1 1.156(3) .
N2 C2 1.345(3) .
N2 C6 1.358(3) .
N3 N4 1.363(3) .
N3 C7 1.325(3) .
N4 C8 1.314(3) .
N5 N6 1.428(3) .
N5 C7 1.356(3) .
N5 C8 1.369(3) .
N6 H6A 1.00(3) .
N6 H6B 0.90(3) .
N7 C9 1.334(3) .
N7 C10 1.337(3) .
C2 H2 0.9500 .
C2 C3 1.387(4) .
C3 H3 0.9500 .
C3 C4 1.375(4) .
C4 H4 0.9500 .
C4 C5 1.391(4) .
C5 H5 0.9500 .
C5 C6 1.385(3) .
C6 C7 1.449(3) .
C8 C9 1.472(3) .
C9 C13 1.385(4) .
C10 H10 0.9500 .
C10 C11 1.382(4) .
C11 H11 0.9500 .
C11 C12 1.378(4) .
C12 H12 0.9500 .
C12 C13 1.392(4) .
C13 H13 0.9500 .
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
_geom_hbond_publ_flag
N6 H6A Se1 1.00(3) 2.66(3) 3.490(3) 141(2) 4_676 yes
N6 H6B N7 0.90(3) 2.12(3) 2.852(3) 137(3) . yes
C2 H2 N4 0.95 2.39 3.181(3) 140.4 3_666 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
Fe1 N2 C2 C3 -176.67(19)
Fe1 N2 C6 C5 175.0(2)
Fe1 N2 C6 C7 -8.1(3)
Fe1 N3 N4 C8 -176.90(19)
Fe1 N3 C7 N5 177.72(15)
Fe1 N3 C7 C6 2.3(3)
N2 C2 C3 C4 1.3(4)
N2 C6 C7 N3 3.9(3)
N2 C6 C7 N5 -170.3(3)
N3 N4 C8 N5 0.7(3)
N3 N4 C8 C9 -177.7(2)
N4 N3 C7 N5 0.9(3)
N4 N3 C7 C6 -174.6(2)
N4 C8 C9 N7 -173.1(2)
N4 C8 C9 C13 7.7(4)
N5 C8 C9 N7 8.7(4)
N5 C8 C9 C13 -170.5(2)
N6 N5 C7 N3 176.3(2)
N6 N5 C7 C6 -9.1(4)
N6 N5 C8 N4 -176.7(2)
N6 N5 C8 C9 1.6(4)
N7 C9 C13 C12 -1.6(4)
N7 C10 C11 C12 -0.4(4)
C2 N2 C6 C5 -3.3(4)
C2 N2 C6 C7 173.7(2)
C2 C3 C4 C5 -2.0(4)
C3 C4 C5 C6 0.3(4)
C4 C5 C6 N2 2.5(4)
C4 C5 C6 C7 -174.0(2)
C5 C6 C7 N3 -179.3(2)
C5 C6 C7 N5 6.6(5)
C6 N2 C2 C3 1.4(4)
C7 N3 N4 C8 -1.0(3)
C7 N5 C8 N4 -0.2(3)
C7 N5 C8 C9 178.2(2)
C8 N5 C7 N3 -0.4(3)
C8 N5 C7 C6 174.2(3)
C8 C9 C13 C12 177.6(2)
C9 N7 C10 C11 -1.7(4)
C10 N7 C9 C8 -176.4(2)
C10 N7 C9 C13 2.8(4)
C10 C11 C12 C13 1.6(4)
C11 C12 C13 C9 -0.7(4)
