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_7715946
_publ_section_title
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 Spin crossover of a Fe(II) mononuclear complex induced by intermolecular
 factors involving chloride and solvent ordering.
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_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), 1.5(O), C O, 0.8[H2O]'
_chemical_formula_sum            'C36 H42.6 Cl2 Fe N13 O5.3'
_chemical_formula_weight         868.98
_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                   32.168(6)
_cell_length_b                   16.288(3)
_cell_length_c                   20.562(4)
_cell_measurement_reflns_used    2562
_cell_measurement_temperature    100
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      2.39
_cell_volume                     8289(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      100.00
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.794
_diffrn_measurement_device_type  'Australian Synchrotron MX1 Beamline'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.794
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            51901
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.794
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.729
_diffrn_reflns_theta_min         1.497
_exptl_absorpt_coefficient_mu    0.551
_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    1.393
_exptl_crystal_description       block
_exptl_crystal_F_000             3616
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method 'Vapour Diffusion'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.194
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         8539
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0599
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1094P)^2^+18.7559P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1712
_refine_ls_wR_factor_ref         0.1775
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7491
_reflns_number_total             8539
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00706a2.cif
_cod_data_source_block           check_a_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7715944--7715949.cif.'
_cod_original_cell_volume        8289(4)
_cod_original_formula_sum        'C36 H42.60 Cl2 Fe N13 O5.30'
_cod_database_code               7715946
_shelx_shelxl_version_number     2019/1
_olex2_refinement_description
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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
 C5-O5
 1.4 with sigma of 0.01
 O4-C4
 1.4 with sigma of 0.02
 C1-O1
 1.4 with sigma of 0.02
 C5D-O5D
 1.4 with sigma of 0.01
 O5-C5 \\sim C5D-O5D
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C5) = Uanis(C5D)
4. Rigid body (RIGU) restrains
 O4, C4
 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
 O1, C1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O5D, C5D
 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
5. Others
 Sof(C5D)=Sof(H5DA)=Sof(H5DB)=Sof(H5DC)=Sof(O5D)=Sof(H5DD)=1-FVAR(1)
 Sof(O5)=Sof(H5)=Sof(C5)=Sof(H5D)=Sof(H5E)=Sof(H5F)=FVAR(1)
 Fixed Sof: O2(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1B(H1BA,H1BB), C2C(H2CA,H2CB), C2A(H2AA,H2AB), C1C(H1CA,H1CB), C1A(H1AA,
 H1AB), C2B(H2BA,H2BB)
6.b Aromatic/amide H refined with riding coordinates:
 C6B(H6B), C6C(H6C), C6A(H6A), C3B(H3B), C11B(H11B), C5C(H5C), C3A(H3A),
 C3C(H3C), C5B(H5B), C10B(H10B), C5A(H5A), C8A(H8A), C7C(H7C), C8C(H8C),
 C7B(H7B), C7A(H7A), C10C(H10C), C10A(H10A), C8B(H8B), C11A(H11A), C11C(H11C)
6.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5D,H5E,H5F), C5D(H5DA,H5DB,H5DC)
6.d Idealised tetrahedral OH refined as rotating group:
 O4(H4), O5(H5), O5D(H5DD)
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_smtbx_masks_special_details
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A solvent mask was calculated and 68 electrons were 
found in a volume of 224\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.8[H2O] per Asymmetric Unit 
which account for 64 electrons 
per unit cell.
;
_shelx_res_checksum              27684
_shelx_fab_checksum              82403
_olex2_submission_special_instructions 'No special instructions were received'