Structural studies into the spin crossover behaviour of Fe(abpt)2(NCS)2 polymorphs B and D
Mason, Helen E.; Musselle-Sexton, Jake R. C.; Howard, Judith A. K.; Probert, Michael R.; Sparkes, Hazel A.; New Journal of Chemistry 45 (2021) 14014–14023; doi:10.1039/D1NJ02607K

data_7060825
_publ_section_title
;
 Structural studies into the spin crossover behaviour of Fe(abpt)2(NCS)2
 polymorphs B and D
;
_journal_issue                   31
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              14014
_journal_page_last               14023
_journal_paper_doi               10.1039/D1NJ02607K
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         '2(C13 H10 Fe0.5 N7 S)'
_chemical_formula_sum            'C26 H20 Fe N14 S2'
_chemical_formula_weight         648.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2021-03-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-05-27 deposited with the CCDC.	2021-07-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.721(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.760(2)
_cell_length_b                   15.808(6)
_cell_length_c                   17.253(4)
_cell_measurement_reflns_used    6977
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      38.635
_cell_measurement_theta_min      5.154
_cell_volume                     2810.5(14)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX2 (Bruker 2013)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.545
_diffrn_measured_fraction_theta_max 0.545
_diffrn_measurement_device       'four-circle Huber diffractometer'
_diffrn_measurement_device_type  'Bruker APEX2 area detector'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_Laue_measured_fraction_full 0.545
_diffrn_reflns_Laue_measured_fraction_max 0.545
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23079
_diffrn_reflns_point_group_measured_fraction_full 0.545
_diffrn_reflns_point_group_measured_fraction_max 0.545
_diffrn_reflns_theta_full        19.536
_diffrn_reflns_theta_max         19.536
_diffrn_reflns_theta_min         1.559
_diffrn_source                   'microfocus sealed X-ray tube Ag'
_diffrn_source_current           0.6
_diffrn_source_power             0.03
_diffrn_source_type              'Incoatec I\ms Ag'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.382
_exptl_absorpt_correction_T_max  0.7444
_exptl_absorpt_correction_T_min  0.6216
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016) was used for absorption correction.'
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_description       block
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.262
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         2717
_refine_ls_number_restraints     351
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0353P)^2^+3.5677P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.1028
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2070
_reflns_number_total             2717
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj02607k2.cif
_cod_data_source_block           polyd_1_8kbar
_cod_depositor_comments
'Adding full bibliography for 7060820--7060846.cif.'
_cod_database_code               7060825
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Restrained distances
 S2-C14 \\sim S2A-C14
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(S2) = Uanis(S2A)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(S2A)=1-FVAR(1)
 Sof(S2)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C15(H15), C16(H16), C17(H17), C18(H18),
 C23(H23), C24(H24), C25(H25), C26(H26), C13(H13), C12(H12), C10(H10), C11(H11)
;
_shelx_res_checksum              75479
_olex2_exptl_crystal_mounting_method
'crystal was mounted inside a diamond anvil cell with a small ruby chip.'
_olex2_submission_special_instructions 'No special instructions were received'