Structural and spectroscopic characterisation of the spin crossover in [Fe(abpt)2(NCS)2] polymorph A
Mason, Helen E.; Li, Wei; Carpenter, Michael A.; Hamilton, Michelle L.; Howard, Judith A. K.; Sparkes, Hazel A.; New J. Chem. 40 (2016) 2466–; doi:10.1039/C5NJ02359A

data_7055291
_publ_section_title
;
 Structural and spectroscopic characterisation of the spin crossover in
 [Fe(abpt)2(NCS)2] polymorph A
;
_journal_issue                   3
_journal_name_full               'New J. Chem.'
_journal_page_first              2466
_journal_paper_doi               10.1039/C5NJ02359A
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         'C26 H20 Fe N14 S2'
_chemical_formula_sum            'C26 H20 Fe N14 S2'
_chemical_formula_weight         648.53
_chemical_name_systematic
bis(4-amino-3,5-bis(pyridin-2-yl)-1,2,4-triazole)-bis(isothiocyanato)-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
_audit_creation_date             2014-11-24
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.11.21 svn.r3092 for OlexSys, GUI svn.r4949)
;
_audit_update_record
;
2015-09-03 deposited with the CCDC.
2016-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.414(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.3440(15)
_cell_length_b                   9.955(3)
_cell_length_c                   15.960(3)
_cell_measurement_reflns_used    2174
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      19.783
_cell_measurement_theta_min      3.296
_cell_volume                     1323.4(5)
_computing_cell_refinement       'APEX2 (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'APEX2 SAINT+ V8.32B (Bruker, 2013)'
_computing_molecular_graphics
'ORTEP-3 for Windows (L. J. Farrugia, WinGX and ORTEP for Windows: an update, J. Appl. Cryst. (2012), 45, 849-854)'
_computing_publication_material
"'WinGX publication routines (L. J. Farrugia, WinGX and ORTEP for Windows: an update, J. Appl. Cryst. (2012),45, 849-854), Olex2 (O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,"
_computing_structure_refinement
'SHELXL-2013 (G. M. Sheldrick, A short history of SHELX, Acta Cryst. (2008), A64, 112-122)'
_computing_structure_solution
'SHELXS-2013 (G. M. Sheldrick, A short history of SHELX, Acta Cryst. (2008), A64, 112-122)'
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEXII CCD area detector'
_diffrn_measured_fraction_theta_full 0.329
_diffrn_measured_fraction_theta_max 0.329
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_collimation    'Multilayer mirrors'
_diffrn_radiation_monochromator  'Bruker Helios multilayer mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 0.329
_diffrn_reflns_Laue_measured_fraction_max 0.329
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            4597
_diffrn_reflns_point_group_measured_fraction_full 0.329
_diffrn_reflns_point_group_measured_fraction_max 0.329
_diffrn_reflns_theta_full        19.742
_diffrn_reflns_theta_max         19.742
_diffrn_reflns_theta_min         2.017
_diffrn_source                   'Microfocus sealed tube'
_diffrn_source_target            Ag
_diffrn_source_type              'Incoatec IuS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.409
_exptl_absorpt_correction_T_max  0.9280
_exptl_absorpt_correction_T_min  0.8120
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0538 before and 0.0390 after correction.
The Ratio of minimum to maximum transmission is 0.8750.
The \l/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    1.627
_exptl_crystal_description       block
_exptl_crystal_F_000             664
_exptl_crystal_preparation
'Slow diffusion of abpt ligand in methanol solution into 1:1 methanol:water Fe2+/2(NCS-) solution.'
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.118
_refine_diff_density_min         -0.103
_refine_diff_density_rms         0.027
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         794
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0229
_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/[\s^2^(Fo^2^)+(0.0214P)^2^+0.7796P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0492
_refine_ls_wR_factor_ref         0.0530
_reflns_Friedel_coverage         0.000
_reflns_number_gt                681
_reflns_number_total             794
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj02359a2.cif
_cod_data_source_block           5kbar
_cod_depositor_comments
'Adding full bibliography for 7055281--7055291.cif.'
_cod_database_code               7055291
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.934
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Restrained distances
 N6-H6A
 0.861 with sigma of 0.02
 N6-H6B
 0.861 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12), C13(H13)
;
_shelx_res_checksum              72868
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'