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_7703916
_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, 7[CH3OH], 1[H2O]'
_chemical_formula_sum            'C67 H84 B2 Fe3 N22 O8'
_chemical_formula_weight         1514.73
_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             2020-03-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-28 deposited with the CCDC.	2020-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.646(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.309(4)
_cell_length_b                   18.909(4)
_cell_length_c                   23.215(4)
_cell_measurement_reflns_used    9855
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      24.717
_cell_measurement_theta_min      2.357
_cell_volume                     7764(3)
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      299.97
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0475
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            33317
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        24.797
_diffrn_reflns_theta_max         24.797
_diffrn_reflns_theta_min         2.154
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.618
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6025
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1239 before and 0.0651 after correction. The Ratio of minimum to maximum transmission is 0.8086. 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             3168
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.481
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         6644
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0614P)^2^+15.5211P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1379
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5045
_reflns_number_total             6644
_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               7703916
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.930
_shelx_estimated_absorpt_t_min   0.876
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
 C16, C15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C16, C17
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C14, C15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C14, C13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C13, C12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C15 \\sim C16: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C16 \\sim C17: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C14 \\sim C15: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C14 \\sim C13: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C13 \\sim C12: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C18(H18A,H18B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C9(H9), C14(H14), C11(H11), C12(H12),
 C13(H13), C16(H16), C17(H17), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26),
  C27(H27), C28(H28), C29(H29), C30(H30)
;
_shelx_res_checksum              12706
_shelx_fab_checksum              40597
_olex2_submission_special_instructions 'No special instructions were received'