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_7703920
_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, 2(C H2 Cl2), 5(C H4 O)'
_chemical_formula_sum            'C73 H90 B2 Cl4 Fe3 N22 O5'
_chemical_formula_weight         1686.63
_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
_atom_sites_solution_primary     iterative
_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                 113.46
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.4576(12)
_cell_length_b                   20.1964(13)
_cell_length_c                   23.1855(12)
_cell_measurement_reflns_used    7341
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.663
_cell_measurement_theta_min      2.822
_cell_volume                     7928.6(8)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0538
_diffrn_reflns_av_unetI/netI     0.0449
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            28328
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        24.818
_diffrn_reflns_theta_max         24.818
_diffrn_reflns_theta_min         2.233
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.741
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6642
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0801 before and 0.0552 after correction. The Ratio of minimum to maximum transmission is 0.8914. 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    1.413
_exptl_crystal_description       block
_exptl_crystal_F_000             3512
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.947
_refine_diff_density_min         -1.023
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         6788
_refine_ls_number_restraints     195
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0754
_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^)+(0.0977P)^2^+48.3672P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1937
_refine_ls_wR_factor_ref         0.2095
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5288
_reflns_number_total             6788
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00016g2.cif
_cod_data_source_block           Tp3Me_100K
_cod_depositor_comments
'Adding full bibliography for 7703915--7703920.cif.'
_cod_original_cell_volume        7928.8(8)
_cod_database_code               7703920
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, 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, All C(H,H,H,H,H,H) groups, All O(H) groups
2. Restrained distances
 O2B-C35B = O2A-C35A
 1.42 with sigma of 0.02
 Cl1B-C37A = Cl2B-C37B = Cl2A-C37B = Cl1A-C37A
 1.79 with sigma of 0.02
 O3-C36
 1.42 with sigma of 0.02
 O1B-C34
 1.45 with sigma of 0.02
 Cl1B-Cl1A = Cl2B-Cl2A
 2.9 with sigma of 0.04
3. Rigid bond restraints
 C17, C8, C9, C10, C11, C16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C11, C16, C15, C14, C13, C12
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
O2B \\sim C35B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
Cl1A \\sim Cl1B \\sim Cl2A \\sim Cl2B \\sim O3 \\sim C36 \\sim C37A \\sim C37B:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
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(C13) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C16)
\\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C14) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.04
Uanis(Cl1B) \\sim Ueq, Uanis(C37A) \\sim Ueq, Uanis(Cl1A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C35B) \\sim Ueq, Uanis(O2B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C37A) = Uanis(C37B)
Uanis(Cl1B) = Uanis(Cl2B)
Uanis(O1A) = Uanis(O1B)
Uanis(O2A) = Uanis(O2B)
Uanis(C35A) = Uanis(C35B)
Uanis(Cl1A) = Uanis(Cl2A)
5. 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)
 Sof(Cl2A)=Sof(Cl2B)=Sof(C37B)=Sof(H37C)=Sof(H37D)=1-FVAR(2)
 Sof(Cl1A)=Sof(Cl1B)=Sof(C37A)=Sof(H37A)=Sof(H37B)=FVAR(2)
 Sof(O1B)=Sof(H1B)=Sof(H34D)=Sof(H34E)=Sof(H34F)=1-FVAR(3)
 Sof(O1A)=Sof(H1AA)=Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(3)
 Sof(O2B)=Sof(H2B)=Sof(C35B)=Sof(H35D)=Sof(H35E)=Sof(H35F)=1-FVAR(4)
 Sof(O2A)=Sof(H2A)=Sof(C35A)=Sof(H35A)=Sof(H35B)=Sof(H35C)=FVAR(4)
 Fixed Sof: O3(0.5) H3A(0.5) C36(0.5) H36A(0.5) H36B(0.5) H36C(0.5)
6.a Ternary CH refined with riding coordinates:
 B1(H1A)
6.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7AA,H7AB), C7(H7BC,H7BD), C18(H18A,H18B), C37A(H37A,H37B),
 C37B(H37C,H37D)
6.c Me refined with everything fixed:
 C34(H34A,H34B,H34C), C34(H34D,H34E,H34F), C36(H36A,H36B,H36C)
6.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), 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), C22(H22), C23(H23), C26(H26), C27(H27), C30(H30),
  C31(H31)
6.e 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)
6.f Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C29(H29A,H29B,H29C), C33(H33A,H33B,H33C), C35A(H35A,H35B,
 H35C), C35B(H35D,H35E,H35F)
6.g Idealised tetrahedral OH refined with riding coordinates:
 O3(H3A)
6.h Idealised tetrahedral OH refined as rotating group:
 O1A(H1AA), O1B(H1B), O2A(H2A), O2B(H2B)
;
_shelx_res_checksum              74359
_olex2_submission_special_instructions 'No special instructions were received'