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_7717105
_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 H36 N, C2 H3 N4, 3(C3 H4 N2)'
_chemical_formula_sum            'C27 H51 N11'
_chemical_formula_weight         529.79
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-97
_audit_update_record
;
2024-07-15 deposited with the CCDC.	2024-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.447(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.7821(4)
_cell_length_b                   8.2254(4)
_cell_length_c                   19.3571(7)
_cell_measurement_reflns_used    7892
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.7800
_cell_measurement_theta_min      4.5440
_cell_volume                     1557.01(11)
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_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  0.0445
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12397
_diffrn_reflns_point_group_measured_fraction_full 0.668
_diffrn_reflns_point_group_measured_fraction_max 0.668
_diffrn_reflns_theta_full        66.570
_diffrn_reflns_theta_max         66.570
_diffrn_reflns_theta_min         4.522
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.561
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49458
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.120a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.130
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.183
_refine_diff_density_min         -0.151
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.1(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         3685
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0617P)^2^+0.1914P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.0998
_reflns_Friedel_coverage         0.336
_reflns_Friedel_fraction_full    0.337
_reflns_Friedel_fraction_max     0.337
_reflns_number_gt                3390
_reflns_number_total             3685
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02244k2.cif
_cod_data_source_block           OH153
_cod_depositor_comments
'Adding full bibliography for 7717105--7717112.cif.'
_cod_original_sg_symbol_Hall     ' 	P -2yc '
_cod_original_sg_symbol_H-M      'P 1 c 1 '
_cod_database_code               7717105
_shelx_res_checksum              92213
_shelx_hkl_checksum              29629