Gradual spin crossover behavior encompasing room temperature in an iron(II) complex based on a heteroscorpionate ligand.
Horniichuk, Oleksandr Ye; Vendier, Laure; Salmon, Lionel; Bousseksou, Azzedine; Dalton transactions (Cambridge, England : 2003) 53 (2024) 17083–17096; doi:10.1039/d4dt02244k

data_7717107
_publ_section_title
;
 Gradual spin crossover behavior encompasing room temperature in an
 iron(II) complex based on a heteroscorpionate ligand.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17083
_journal_page_last               17096
_journal_paper_doi               10.1039/d4dt02244k
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C16 H20 B2 Fe N16'
_chemical_formula_sum            'C16 H20 B2 Fe N16'
_chemical_formula_weight         513.92
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_update_record
;
2024-07-18 deposited with the CCDC.	2024-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.662(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6457(2)
_cell_length_b                   16.6839(5)
_cell_length_c                   13.0720(3)
_cell_measurement_reflns_used    7649
_cell_measurement_temperature    393
_cell_measurement_theta_max      76.39
_cell_measurement_theta_min      4.29
_cell_volume                     2314.06(10)
_computing_cell_refinement
; 
 CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)
;
_computing_data_collection       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_reduction
; 
 CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)
;
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      393
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.031
_diffrn_reflns_av_unetI/netI     0.048
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18004
_diffrn_reflns_theta_full        66.9692
_diffrn_reflns_theta_max         77.509
_diffrn_reflns_theta_min         4.306
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.584
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.81
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.46
_refine_diff_density_min         -0.74
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0248
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         4321
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.0061984
_refine_ls_shift/su_mean         0.0002847
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.08P)^2^ + 1.82P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1498
_refine_ls_wR_factor_gt          0.1427
_refine_ls_wR_factor_ref         0.1498
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                3557
_reflns_number_total             4588
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0572
_oxford_refine_ls_scale          0.3953(8)
_oxford_reflns_number_all        4321
_cod_data_source_file            d4dt02244k2.cif
_cod_data_source_block           OH184-393K
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7717105--7717112.cif.
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               7717107
_oxford_refine_reflns_threshold_expression I>-3.0\s(I)
_oxford_refine_ls_r_factor_all   0.0572
_oxford_refine_ls_wr_factor_all  0.1498