Slow magnetic relaxation in a trigonal-planar mononuclear Fe(ii) complex
Li, Yuzhu; Xi, Jing; Ferrando-Soria, Jesús; Zhang, Yi-Quan; Wang, Wenyuan; Song, You; Guo, Yan; Pardo, Emilio; Liu, Xiangyu; Dalton Transactions  (2022) –; doi:10.1039/D2DT00899H

data_7710282
_publ_section_title
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 Slow magnetic relaxation in a trigonal-planar mononuclear Fe(ii) complex
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00899H
_journal_year                    2022
_chemical_formula_moiety         'C45 H49 Cl Fe N2'
_chemical_formula_sum            'C45 H49 Cl Fe N2'
_chemical_formula_weight         709.16
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-11-04 deposited with the CCDC.	2022-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3687(7)
_cell_length_b                   22.9892(10)
_cell_length_c                   13.9721(6)
_cell_measurement_reflns_used    9838
_cell_measurement_temperature    153.15
_cell_measurement_theta_max      26.114
_cell_measurement_theta_min      2.199
_cell_volume                     3972.9(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      153.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1450
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            75142
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.423
_diffrn_reflns_theta_min         2.199
_exptl_absorpt_coefficient_mu    0.479
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6131
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1878 before and 0.1005 after correction. The Ratio of minimum to maximum transmission is 0.8225. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.901
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         4187
_refine_ls_number_restraints     186
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0598
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1036P)^2^+3.3323P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1777
_refine_ls_wR_factor_ref         0.1932
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2994
_reflns_number_total             4187
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00899h2.cif
_cod_data_source_block           guoyan20190308
_cod_database_code               7710282
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.954
_shelx_estimated_absorpt_t_min   0.932
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C19A \\sim C20A \\sim C21A \\sim C22A \\sim C22 \\sim C23 \\sim C23A \\sim C19
\\sim C24A \\sim C24 \\sim C20 \\sim C21: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
3. Others
 Sof(C19A)=Sof(C24A)=Sof(H24A)=Sof(C23A)=Sof(H23A)=Sof(C22A)=Sof(H22A)=
 Sof(C21A)=Sof(H21A)=Sof(C20A)=Sof(H20A)=1-FVAR(1)
 Sof(C19)=Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21)=Sof(C22)=Sof(H22)=Sof(C23)=
 Sof(H23)=Sof(C24)=Sof(H24)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C8(H8), C17(H17)
4.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C20(H20), C21(H21), C22(H22), C23(H23),
 C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C24A(H24A),
 C23A(H23A), C22A(H22A), C21A(H21A), C20A(H20A)
4.c Fitted hexagon refined as free rotating group:
 C19A(C24A,C23A,C22A,C21A,C20A)
4.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              74639
_olex2_submission_special_instructions 'No special instructions were received'