[Fe(abpt)2(NCSe)2] polymorph A: structural studies into the spin crossover behaviour
Mason, Helen E.; Hamilton, Michelle L.; Howard, Judith A. K.; Sparkes, Hazel A.; New Journal of Chemistry 42 (2018) 18028–; doi:10.1039/C8NJ03627F

data_7057797
_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             2017-06-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-07-19 deposited with the CCDC.
2018-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.1310(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.4815(4)
_cell_length_b                   9.9987(5)
_cell_length_c                   16.3984(9)
_cell_measurement_reflns_used    5124
_cell_measurement_temperature    175(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.39
_cell_volume                     1388.57(12)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      175(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 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 1K area detector'
_diffrn_measurement_method       '\w 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  0.0303
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9355
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.278
_diffrn_reflns_theta_min         2.387
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.211
_exptl_absorpt_correction_T_max  0.6305
_exptl_absorpt_correction_T_min  0.4879
_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 0.0692 before and 0.0452 
after correction. The Ratio of minimum to maximum transmission is 
0.7738. 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    1.775
_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         0.746
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         3444
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0231P)^2^+1.5390P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0739
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2864
_reflns_number_total             3444
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj03627f2.cif
_cod_data_source_block           175K
_cod_depositor_comments
'Adding full bibliography for 7057796--7057812.cif.'
_cod_database_code               7057797
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.628
_shelx_estimated_absorpt_t_min   0.489
_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
 0.96 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              84493
_shelx_hkl_checksum              80544
_olex2_exptl_crystal_mounting_method
'Glued onto a glass fibre using epoxy adhesive'
_olex2_submission_original_sample_id 13HM087
_olex2_submission_special_instructions 'No special instructions were received'