Manipulating the spin crossover behavior in a series of {FeFe<sup>II</sup>} complexes.
Chen, Jia-Tao; Zhao, Xin-Hua; Zhang, Yuan-Zhu; Dalton transactions (Cambridge, England : 2003) 49 (2020) 5949–5956; doi:10.1039/d0dt00016g

data_7703918
_publ_section_title
;
 Manipulating the spin crossover behavior in a series of
 {FeFe<sup>II</sup>} complexes.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5949
_journal_page_last               5956
_journal_paper_doi               10.1039/d0dt00016g
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C66 H66 B2 Fe3 N22, 3[CH3OH], 2[CH2Cl2]'
_chemical_formula_sum            'C71 H82 B2 Cl4 Fe3 N22 O3'
_chemical_formula_weight         1622.55
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-27 deposited with the CCDC.	2020-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.627(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.936(6)
_cell_length_b                   20.261(6)
_cell_length_c                   23.361(5)
_cell_measurement_reflns_used    7054
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      24.563
_cell_measurement_theta_min      2.348
_cell_volume                     8211(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      300.02
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0933
_diffrn_reflns_av_unetI/netI     0.0825
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            25887
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        24.792
_diffrn_reflns_theta_max         24.792
_diffrn_reflns_theta_min         2.224
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.711
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6321
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1565 before and 0.0737 after correction. The Ratio of minimum to maximum transmission is 0.8483. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_description       block
_exptl_crystal_F_000             3368
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         7032
_refine_ls_number_restraints     83
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1053
_refine_ls_R_factor_gt           0.0704
_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^)+(0.0937P)^2^+16.2862P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1792
_refine_ls_wR_factor_ref         0.1948
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4840
_reflns_number_total             7032
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00016g2.cif
_cod_data_source_block           Tp3Me_300K
_cod_depositor_comments
'Adding full bibliography for 7703915--7703920.cif.'
_cod_database_code               7703918
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C11, C16, C17, C8, C9, C10
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C14, C13, C12, C11, C16, C15
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C11) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.04
Uanis(C14) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C11)
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.04
4. Others
 Sof(H7BC)=Sof(H7BD)=Sof(C17)=Sof(H17)=Sof(C8)=Sof(C9)=Sof(H9)=Sof(C10)=
 Sof(H10)=Sof(C11)=Sof(C16)=Sof(C15)=Sof(H15)=Sof(C14)=Sof(H14)=Sof(C13)=
 Sof(H13)=Sof(C12)=Sof(H12)=1-FVAR(1)
 Sof(H7AA)=Sof(H7AB)=Sof(C9A)=Sof(H9A)=Sof(C8A)=Sof(C17A)=Sof(H17A)=Sof(C16A)=
 Sof(H16A)=Sof(C15A)=Sof(C10A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(H12A)=
 Sof(C13A)=Sof(H13A)=Sof(C14A)=Sof(H14A)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C18(H18A,H18B), C7(H7AA,H7AB), C7(H7BC,H7BD)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C22(H22), C3(H3), C23(H23), C30(H30), C26(H26),
 C31(H31), C27(H27), C9A(H9A), C17A(H17A), C16A(H16A), C11A(H11A), C12A(H12A),
 C13A(H13A), C14A(H14A), C17(H17), C9(H9), C10(H10), C15(H15), C14(H14),
 C13(H13), C12(H12)
5.c Naphthalene refined as free rotating group:
 C9A(C8A,C17A,C16A,C15A,C10A,C11A,C12A,C13A,C14A), C17(C8,C9,C10,C11,C16,C15,
 C14,C13,C12)
5.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C33(H33A,H33B,H33C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              94146
_shelx_fab_checksum              21690
_olex2_submission_special_instructions 'No special instructions were received'