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_7703919
_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         'C72 H78 B2 Fe3 N22, 8(H2 O), 6(C H4 O)'
_chemical_formula_sum            'C78 H118 B2 Fe3 N22 O14'
_chemical_formula_weight         1777.11
_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     iterative
_audit_creation_date             2020-03-10
_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                 114.754(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.0454(12)
_cell_length_b                   19.9288(12)
_cell_length_c                   21.8359(11)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.302
_cell_measurement_theta_min      2.288
_cell_volume                     9107.0(9)
_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      100.02
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_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  0.0832
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            70340
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.472
_diffrn_reflns_theta_min         2.287
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.542
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6323
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0932 before and 0.0680 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    1.296
_exptl_crystal_description       block
_exptl_crystal_F_000             3760
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.691
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         9355
_refine_ls_number_restraints     128
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1153
_refine_ls_R_factor_gt           0.0719
_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^)+(0.1127P)^2^+44.4412P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1948
_refine_ls_wR_factor_ref         0.2408
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6220
_reflns_number_total             9355
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00016g2.cif
_cod_data_source_block           Tpstar_100K
_cod_depositor_comments
'Adding full bibliography for 7703915--7703920.cif.'
_cod_database_code               7703919
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.948
_shelx_estimated_absorpt_t_min   0.923
_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 O(H) groups, All O(H,H) groups
2. Restrained distances
 O3B-C39B
 1.45 with sigma of 0.02
 C39A-O3A
 1.45 with sigma of 0.02
 O3A-C39A
 1.45 with sigma of 0.02
 H1B-H5A
 2.1 with sigma of 0.02
 H8B-H8B_$1
 2.1 with sigma of 0.01
 H8B_$4-H5B
 2.1 with sigma of 0.02
3. Rigid bond restraints
 O1, C37
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 O2, C38
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
O1 \\sim C37: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
C14 \\sim C12 \\sim C11 \\sim C13 \\sim C9 \\sim C8 \\sim C17 \\sim C16 \\sim
C15 \\sim C10: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
O2 \\sim C38: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O3B) \\sim Ueq, Uanis(C39B) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(O7) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O6B) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O3A) \\sim Ueq, Uanis(C39A) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(O4) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C8A) = Uanis(C8)
Uanis(C17) = Uanis(C9A)
Uanis(C17A) = Uanis(C9)
Uanis(C16) = Uanis(C10A)
Uanis(C16A) = Uanis(C10)
Uanis(C15) = Uanis(C11A)
Uanis(C15A) = Uanis(C11)
Uanis(C14) = Uanis(C12A)
Uanis(C14A) = Uanis(C12)
Uanis(C13A) = Uanis(C13)
Uanis(O3A) = Uanis(O3B)
Uanis(C39A) = Uanis(C39B)
5. Others
 Sof(H7BC)=Sof(H7BD)=Sof(C15A)=Sof(H15A)=Sof(C14A)=Sof(H14A)=Sof(C13A)=
 Sof(H13A)=Sof(C12A)=Sof(H12A)=Sof(C11A)=Sof(C16A)=Sof(C17A)=Sof(H17A)=Sof(C8A)=
 Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10A)=1-FVAR(1)
 Sof(H7AA)=Sof(H7AB)=Sof(C9)=Sof(H9)=Sof(C8)=Sof(C17)=Sof(H17)=Sof(C16)=
 Sof(H16)=Sof(C15)=Sof(C10)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(H12)=Sof(C13)=
 Sof(H13)=Sof(C14)=Sof(H14)=FVAR(1)
 Sof(O3B)=Sof(H3B)=Sof(C39B)=Sof(H39D)=Sof(H39E)=Sof(H39F)=1-FVAR(2)
 Sof(O3A)=Sof(H3A)=Sof(C39A)=Sof(H39A)=Sof(H39B)=Sof(H39C)=FVAR(2)
 Sof(O6B)=Sof(H6BA)=Sof(H6BB)=1-FVAR(3)
 Sof(O6A)=Sof(H6AA)=Sof(H6AB)=FVAR(3)
 Fixed Sof: O4(0.5) H4A(0.5) H4B(0.5) O7(0.5) H7A(0.5) H7B(0.5)
6.a Riding coordinates:
 O4(H4A,H4B), O8(H8A,H8B), O2(H2A), O6B(H6BA,H6BB), O3A(H3A), O7(H7A,H7B),
 C39A(H39A,H39B,H39C), C38(H38A,H38B,H38C)
6.b Free rotating group:
 O6A(H6AA,H6AB), O5(H5A,H5B)
6.c Ternary CH refined with riding coordinates:
 B1(H1A)
6.d Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C6(H6A,H6B), C7(H7AA,H7AB), C7(H7BC,H7BD)
6.e Aromatic/amide H refined with riding coordinates:
 C29(H29), C1(H1), C2(H2), C3(H3), C4(H4), C24(H24), C9(H9), C17(H17),
 C16(H16), C11(H11), C12(H12), C13(H13), C14(H14), C34(H34), C15A(H15A),
 C14A(H14A), C13A(H13A), C12A(H12A), C17A(H17A), C9A(H9A), C10A(H10A)
6.f Naphthalene refined as free rotating group:
 C9(C8,C17,C16,C15,C10,C11,C12,C13,C14), C15A(C14A,C13A,C12A,C11A,C16A,C17A,
 C8A,C9A,C10A)
6.g Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C37(H37A,H37B,
 H37C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C36(H36A,H36B,H36C),
 C39B(H39D,H39E,H39F)
6.h Idealised tetrahedral OH refined as rotating group:
 O1(H1B), O3B(H3B)
;
_shelx_res_checksum              19424
_olex2_submission_special_instructions 'No special instructions were received'