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_7055289
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2014-12-04
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_audit_update_record
;
2015-09-03 deposited with the CCDC.
2016-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.978(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.552(3)
_cell_length_b                   10.236(6)
_cell_length_c                   16.444(6)
_cell_measurement_reflns_used    216
_cell_measurement_temperature    296.15(2)
_cell_measurement_theta_max      17.683
_cell_measurement_theta_min      3.333
_cell_volume                     1436.0(11)
_computing_cell_refinement       'APEX2 (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'APEX2 SAINT+ V8.32B (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_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 0.202
_diffrn_measured_fraction_theta_max 0.396
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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  0.0343
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_Laue_measured_fraction_full 0.202
_diffrn_reflns_Laue_measured_fraction_max 0.396
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9085
_diffrn_reflns_point_group_measured_fraction_full 0.202
_diffrn_reflns_point_group_measured_fraction_max 0.396
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         20.502
_diffrn_reflns_theta_min         1.959
_diffrn_source                   'Microfocus sealed tube'
_diffrn_source_target            Ag
_diffrn_source_type              'Incoatec IuS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.377
_exptl_absorpt_correction_T_max  0.9280
_exptl_absorpt_correction_T_min  0.7454
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.500
_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         0.194
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         1158
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0238P)^2^+3.3012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1098
_reflns_Friedel_coverage         0.000
_reflns_number_gt                897
_reflns_number_total             1158
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj02359a2.cif
_cod_data_source_block           ambientpressure
_cod_depositor_comments
'Adding full bibliography for 7055281--7055291.cif.'
_cod_original_cell_volume        1435.9(10)
_cod_database_code               7055289
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.963
_shelx_estimated_absorpt_t_min   0.939
_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              52324
_olex2_exptl_crystal_mounting_method
'diamond anvil cell with paraffin as hydrostatic medium'
_olex2_submission_original_sample_id 13HM001
_olex2_submission_special_instructions 'No special instructions were received'