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_7703915
_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
'C60 H54 B2 Fe3 N22, 4(C H4 O), 0.5(H4 O2), 3[CH3OH]'
_chemical_formula_sum            'C67 H84 B2 Fe3 N22 O8'
_chemical_formula_weight         1514.73
_chemical_name_systematic        Fe2FebnbpenTp100k
_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             2020-03-13
_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                 114.0340(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.3698(6)
_cell_length_b                   18.5637(5)
_cell_length_c                   23.0499(7)
_cell_measurement_reflns_used    9339
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.924
_cell_measurement_theta_min      2.844
_cell_volume                     7569.6(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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      99.99
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.984
_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  0.0379
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            48628
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.940
_diffrn_reflns_theta_min         2.398
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.634
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6575
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0898 before and 0.0486 after correction. The Ratio of minimum to maximum transmission is 0.8818. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_description       block
_exptl_crystal_F_000             3168
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.012
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.799
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         8955
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0443
_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^)+(0.0409P)^2^+19.9420P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1083
_refine_ls_wR_factor_ref         0.1129
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7981
_reflns_number_total             8955
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00016g2.cif
_cod_data_source_block           Tp_100K
_cod_depositor_comments
'Adding full bibliography for 7703915--7703920.cif.'
_cod_database_code               7703915
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.987
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(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
 O1B-C31B = O1A-C31A
 1.45 with sigma of 0.02
 O4-C34 = O1C-C31C
 1.45 with sigma of 0.02
3. Rigid bond restraints
 C11, C12, C13, C14, C15, C16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C13, C14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
C13 \\sim C14: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01
Uanis(C34) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O1C) \\sim Ueq, Uanis(C31C)
\\sim Ueq, Uanis(O1A) \\sim Ueq, Uanis(C31A) \\sim Ueq, Uanis(C31B) \\sim Ueq,
Uanis(O1B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C31B) \\sim Ueq, Uanis(C31A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O1A) = Uanis(O1B)
Uanis(C31A) = Uanis(C31B)
Uanis(O4) = Uanis(O1C)
Uanis(C34) = Uanis(C31C)
5. Others
 1*[Sof(O1A)+Sof(H1AA)+Sof(C31A)+Sof(H31A)+Sof(H31B)+Sof(H31C)]+1*[Sof(O1B)+
 Sof(H1B)+Sof(C31B)+Sof(H31D)+Sof(H31E)+Sof(H31F)]+1*[Sof(O1C)+Sof(H1C)+
 Sof(C31C)+Sof(H31G)+Sof(H31H)+Sof(H31I)]=1 with esd of 0
 Sof(O1A)=Sof(H1AA)=Sof(C31A)=Sof(H31A)=Sof(H31B)=Sof(H31C)=FVAR(1)
 Sof(O1B)=Sof(H1B)=Sof(C31B)=Sof(H31D)=Sof(H31E)=Sof(H31F)=FVAR(2)
 Sof(O1C)=Sof(H1C)=Sof(C31C)=Sof(H31G)=Sof(H31H)=Sof(H31I)=FVAR(3)
 Fixed Sof: O4(0.5) H4A(0.5) H5A(0.5) H5B(0.5) C34(0.5) H34A(0.5) H34B(0.5)
 H34C(0.5)
6.a Free rotating group:
 O5(H5A,H5B)
6.b Ternary CH refined with riding coordinates:
 B1(H1A)
6.c Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C18(H18A,H18B)
6.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27),
  C28(H28), C29(H29), C30(H30)
6.e Idealised Me refined as rotating group:
 C31A(H31A,H31B,H31C), C31B(H31D,H31E,H31F), C31C(H31G,H31H,H31I), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C)
6.f Idealised tetrahedral OH refined as rotating group:
 O1A(H1AA), O1B(H1B), O1C(H1C), O2(H2A), O3(H3A), O4(H4A)
;
_shelx_res_checksum              35018
_olex2_submission_special_instructions 'No special instructions were received'