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_7703917
_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, 6[CH3OH], 8[H2O]'
_chemical_formula_sum            'C78 H118 B2 Fe3 N22 O14'
_chemical_formula_weight         1777.11
_chemical_name_systematic        bnbpenTp+300k
_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     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                 116.701(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.678(7)
_cell_length_b                   21.345(8)
_cell_length_c                   22.221(9)
_cell_measurement_reflns_used    8612
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.070
_cell_measurement_theta_min      2.575
_cell_volume                     10033(6)
_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      100.02
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.973
_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  0.0534
_diffrn_reflns_av_unetI/netI     0.0850
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22160
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.454
_diffrn_reflns_theta_min         2.167
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.492
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6094
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1316 before and 0.0705 after correction. The Ratio of minimum to maximum transmission is 0.8175. 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    1.176
_exptl_crystal_description       block
_exptl_crystal_F_000             3760
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.985
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         10080
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1155
_refine_ls_R_factor_gt           0.0658
_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^)+(0.0558P)^2^+19.6436P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1553
_refine_ls_wR_factor_ref         0.1847
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5704
_reflns_number_total             10080
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00016g2.cif
_cod_data_source_block           Tp+_300K
_cod_depositor_comments
'Adding full bibliography for 7703915--7703920.cif.'
_cod_database_code               7703917
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.943
_shelx_estimated_absorpt_t_min   0.908
_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
2. Uiso/Uaniso restraints and constraints
C9 \\sim C8 \\sim C17 \\sim C16 \\sim C15 \\sim C10 \\sim C11 \\sim C12 \\sim
C13 \\sim C14: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C4BA) = Uanis(C9)
Uanis(C10) = Uanis(C9AA)
Uanis(C3) = Uanis(C8)
Uanis(C15) = Uanis(C3BA)
Uanis(C0BA) = Uanis(C17)
Uanis(C16) = Uanis(C4AA)
Uanis(C7AA) = Uanis(C11)
Uanis(C12) = Uanis(C5AA)
Uanis(C2BA) = Uanis(C13)
Uanis(C1BA) = Uanis(C14)
3. Others
 Sof(H7BC)=Sof(H7BD)=Sof(C7AA)=Sof(H7AC)=Sof(C2BA)=Sof(H2BA)=Sof(C1BA)=
 Sof(H1BA)=Sof(C5AA)=Sof(H5AA)=Sof(C4AA)=Sof(C0BA)=Sof(C3)=Sof(H3)=Sof(C4BA)=
 Sof(C9AA)=Sof(H9AA)=Sof(C3BA)=Sof(H3BA)=1-FVAR(1)
 Sof(H7AA)=Sof(H7AB)=Sof(C8)=Sof(H8)=Sof(C9)=Sof(C10)=Sof(H10)=Sof(C15)=
 Sof(H15)=Sof(C16)=Sof(C17)=Sof(C11)=Sof(H11)=Sof(C13)=Sof(H13)=Sof(C14)=
 Sof(H14)=Sof(C12)=Sof(H12)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 B1(H1A)
4.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7AA,H7AB), C7(H7BC,H7BD), C18(H18A,H18B)
4.c Aromatic/amide H refined with riding coordinates:
 C24(H24), C1(H1), C29(H29), C2(H2), C4(H4), C2AA(H2AA), C34(H34), C8(H8),
 C10(H10), C15(H15), C11(H11), C13(H13), C14(H14), C12(H12), C7AA(H7AC),
 C2BA(H2BA), C1BA(H1BA), C5AA(H5AA), C3(H3), C9AA(H9AA), C3BA(H3BA)
4.d Naphthalene refined as free rotating group:
 C8(C9,C10,C15,C16,C17,C11,C13,C14,C12), C7AA(C2BA,C1BA,C5AA,C4AA,C0BA,C3,C4BA,
 C9AA,C3BA)
4.e Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C26(H26A,H26B,H26C), C23(H23A,H23B,H23C), C28(H28A,H28B,
 H28C), C36(H36A,H36B,H36C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              66490
_shelx_fab_checksum              59672
_olex2_submission_special_instructions 'No special instructions were received'