Spin crossover of a Fe(II) mononuclear complex induced by intermolecular factors involving chloride and solvent ordering.
Zhang, Kenneth; Wallis, Matthew J.; Craze, Alexander R.; Hayami, Shinya; Min, Hyunsung; Fanna, Daniel J.; Bhadbhade, Mohan M.; Tian, Ruoming; Marjo, Christopher E.; Lindoy, Leonard F.; Li, Feng; Dalton transactions (Cambridge, England : 2003) 53 (2024) 14144–14152; doi:10.1039/d4dt00706a

data_7715948
_publ_section_title
;
 Spin crossover of a Fe(II) mononuclear complex induced by intermolecular
 factors involving chloride and solvent ordering.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14144
_journal_page_last               14152
_journal_paper_doi               10.1039/d4dt00706a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'C33 H33 Fe N13, 2(Cl), 2.3(C O), H2 O, 0.7[CH4O], 1.3[H2O]'
_chemical_formula_sum            'C36 H40.4 Cl2 Fe N13 O5.3'
_chemical_formula_weight         866.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2024-03-07
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-03-08 deposited with the CCDC.	2024-05-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 129.57(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.450(7)
_cell_length_b                   16.530(3)
_cell_length_c                   20.800(4)
_cell_measurement_reflns_used    2562
_cell_measurement_temperature    250
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      2.39
_cell_volume                     8600(5)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      250.00
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.789
_diffrn_measurement_device_type  MX1
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0147
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.789
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            54313
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.789
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.718
_diffrn_reflns_theta_min         1.477
_exptl_absorpt_coefficient_mu    0.531
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear reddish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_description       block
_exptl_crystal_F_000             3598
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method 'Vapour Diffusion of Diethyl Ether'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.064
_refine_diff_density_min         -0.759
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         8791
_refine_ls_number_restraints     157
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0552
_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^)+(0.1292P)^2^+4.0840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1772
_refine_ls_wR_factor_ref         0.1809
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8063
_reflns_number_total             8791
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00706a2.cif
_cod_data_source_block           check_a_CCDC3
_cod_depositor_comments
'Adding full bibliography for 7715944--7715949.cif.'
_cod_original_cell_volume        8601(4)
_cod_original_formula_sum        'C36 H40.40 Cl2 Fe N13 O5.30'
_cod_database_code               7715948
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.949
_shelx_estimated_absorpt_t_min   0.901
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 N4A-C11A = N4A-C7A
 1.3 with sigma of 0.02
 C7A-C8A = C8A-C9A = C10A-C9A = C11A-C10A
 1.4 with sigma of 0.02
 N4C-C7C = N4C-C11C
 1.3 with sigma of 0.02
 C11C-C10C = C10C-C9C = C8C-C9C = C8C-C7C
 1.4 with sigma of 0.02
 N4B-C7B = N4B-C11B
 1.3 with sigma of 0.02
 C7B-C8B = C8B-C9B = C10B-C9B = C11B-C10B
 1.4 with sigma of 0.02
 O4-C4
 1.4 with sigma of 0.02
 O1-C1
 1.4 with sigma of 0.02
 C1-O1
 1.4 with sigma of 0.02
 O5-C5
 1.4 with sigma of 0.01
 N4A-C9A
 2.8 with sigma of 0.04
 C7A-C10A
 2.7 with sigma of 0.04
 C11A-C8A
 2.7 with sigma of 0.04
 N4C-C9C
 2.8 with sigma of 0.04
 C11C-C8C
 2.7 with sigma of 0.04
 C10C-C7C
 2.7 with sigma of 0.04
 N4B-C9B
 2.8 with sigma of 0.04
 C7B-C10B
 2.7 with sigma of 0.04
 C8B-C11B
 2.7 with sigma of 0.04
3. Restrained planarity
 N4A, C9A, C8A, C7A, C10A, C11A
 with sigma of 0.1
 C9C, N4C, C7C, C8C, C10C, C11C
 with sigma of 0.1
 N4B, C9B, C10B, C11B, C8B, C7B
 with sigma of 0.1
4. Rigid body (RIGU) restrains
 N4A, C9A, C8A, C7A, C10A, C11A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C9C, N4C, C7C, C8C, C10C, C11C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N4B, C9B, C10B, C11B, C8B, C7B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, C1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C4, O4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O5, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O1(0.7) C1(0.7) C5(0.6) O5(0.6)
6.a Free rotating group:
 O3(H3D,H3E)
6.b Secondary CH2 refined with riding coordinates:
 C1B(H1BA,H1BB), C1A(H1AA,H1AB), C1C(H1CA,H1CB), C2C(H2CA,H2CB), C2B(H2BA,
 H2BB), C2A(H2AA,H2AB)
6.c Aromatic/amide H refined with riding coordinates:
 C6C(H6C), C6B(H6B), C3C(H3C), C5C(H5C), C3B(H3B), C3A(H3A), C5A(H5A),
 C6A(H6A), C5B(H5B), C10B(H10B), C8A(H8A), C11B(H11B), C7A(H7A), C7C(H7C),
 C8C(H8C), C10A(H10A), C10C(H10C), C8B(H8B), C11A(H11A), C7B(H7B), C11C(H11C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              75266
_shelx_fab_checksum              44572
_olex2_submission_special_instructions 'No special instructions were received'