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_7715945
_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(C H4 O), O, C O, 1.3[H2O]'
_chemical_formula_sum            'C36 H43.6 Cl2 Fe N13 O5.3'
_chemical_formula_weight         869.99
_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   geom
_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                 129.70(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.341(7)
_cell_length_b                   16.381(3)
_cell_length_c                   20.675(4)
_cell_measurement_reflns_used    2564
_cell_measurement_temperature    200
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      2.39
_cell_volume                     8427(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      200.00
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.791
_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  0.0290
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.791
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            53513
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.791
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.701
_diffrn_reflns_theta_min         1.488
_exptl_absorpt_coefficient_mu    0.542
_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    1.371
_exptl_crystal_description       block
_exptl_crystal_F_000             3624
_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         1.120
_refine_diff_density_min         -0.776
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         8626
_refine_ls_number_restraints     116
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0468
_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^)+(0.0822P)^2^+12.1634P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1352
_refine_ls_wR_factor_ref         0.1363
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8272
_reflns_number_total             8626
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00706a2.cif
_cod_data_source_block           check_a_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7715944--7715949.cif.'
_cod_original_cell_volume        8427(4)
_cod_original_formula_sum        'C36 H43.60 Cl2 Fe N13 O5.30'
_cod_database_code               7715945
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.948
_shelx_estimated_absorpt_t_min   0.899
_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 C(H,H,H) groups, All O(H) groups
2. Restrained distances
 N4A-C7A = N4A-C11A
 1.3 with sigma of 0.02
 C11A-C10A = C10A-C9A = C8A-C9A = C7A-C8A
 1.4 with sigma of 0.02
 N4C-C11C = N4C-C7C
 1.3 with sigma of 0.02
 C7C-C8C = C8C-C9C = C10C-C9C = C11C-C10C
 1.4 with sigma of 0.02
 N4B-C11B = N4B-C7B
 1.3 with sigma of 0.02
 C11B-C10B = C10B-C9B = C8B-C9B = C7B-C8B
 1.4 with sigma of 0.02
 O5-C5
 1.4 with sigma of 0.02
 O5D-C5D
 1.4 with sigma of 0.02
 C1-O1
 1.4 with sigma of 0.02
 O4-C4
 1.4 with sigma of 0.01
 N4A-C9A
 2.8 with sigma of 0.04
 C10A-C7A
 2.7 with sigma of 0.04
 C8A-C11A
 2.7 with sigma of 0.04
 N4C-C9C
 2.8 with sigma of 0.04
 C10C-C7C
 2.7 with sigma of 0.04
 C11C-C8C
 2.7 with sigma of 0.04
 N4B-C9B
 2.8 with sigma of 0.04
 C8B-C11B
 2.7 with sigma of 0.04
 C10B-C7B
 2.7 with sigma of 0.04
 C5-O5 \\sim C5D-O5D
 with sigma of 0.02
3. Restrained planarity
 N4A, C9A, C8A, C10A, C7A, C11A
 with sigma of 0.1
 N4C, C9C, C8C, C7C, C10C, C11C
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
: with sigma of 0.1 and sigma for terminal atoms of 0.2
: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uiso(C5) = Uiso(C5D)
5. Rigid body (RIGU) restrains
 N4A, C9A, C8A, C10A, C7A, C11A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N4C, C9C, C8C, C7C, C10C, C11C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C5D, O5D
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C5, O5
 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
6. Others
 Sof(C5D)=Sof(O5D)=1-FVAR(1)
 Sof(C5)=Sof(O5)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C2B(H2BA,H2BB), C1B(H1BA,H1BB), C2C(H2CA,H2CB), C2A(H2AA,H2AB), C1A(H1AA,
 H1AB), C1C(H1CA,H1CB)
7.b Aromatic/amide H refined with riding coordinates:
 C6B(H6B), C3C(H3C), C3B(H3B), C5C(H5C), C6C(H6C), C3A(H3A), C5B(H5B),
 C6A(H6A), C10B(H10B), C8A(H8A), C11B(H11B), C8C(H8C), C7C(H7C), C5A(H5A),
 C8B(H8B), C10A(H10A), C7A(H7A), C11A(H11A), C10C(H10C), C7B(H7B), C11C(H11C)
7.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C1(H1A,H1B,H1C)
7.d Idealised tetrahedral OH refined as rotating group:
 O4(H4), O1(H1)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              20556
_shelx_fab_checksum              31293
_olex2_submission_special_instructions 'No special instructions were received'