Spin and valence isomerism in cyanide-bridged {FeM<sup>II</sup>} (M = Fe and Co) clusters.
Zhao, Xin-Hua; Shao, Dong; Chen, Jia-Tao; Liu, Min; Li, Tao; Yang, Jiong; Zhang, Yuan-Zhu; Dalton transactions (Cambridge, England : 2003) 50 (2021) 9768–9774; doi:10.1039/d1dt01298c

data_7707649
_publ_section_title
;
 Spin and valence isomerism in cyanide-bridged {FeM<sup>II</sup>} (M = Fe
 and Co) clusters.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9768
_journal_page_last               9774
_journal_paper_doi               10.1039/d1dt01298c
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C63 H73 B2 Fe3 N23, C H4 O, 3(H2 O)'
_chemical_formula_sum            'C64 H83 B2 Fe3 N23 O4'
_chemical_formula_weight         1427.70
_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             2020-04-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-05-13 deposited with the CCDC.	2021-06-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.207(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.462(4)
_cell_length_b                   22.513(4)
_cell_length_c                   16.255(3)
_cell_measurement_reflns_used    9950
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      26.337
_cell_measurement_theta_min      2.597
_cell_volume                     7891(2)
_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      290.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0514
_diffrn_reflns_av_unetI/netI     0.0626
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28350
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.583
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.601
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6092
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0955 before and 0.0576 after correction. The Ratio of minimum to maximum transmission is 0.8173. 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    1.202
_exptl_crystal_description       block
_exptl_crystal_F_000             2992
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         8036
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1238
_refine_ls_R_factor_gt           0.0681
_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^)+(0.1431P)^2^+7.5563P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1986
_refine_ls_wR_factor_ref         0.2491
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4643
_reflns_number_total             8036
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01298c3.cif
_cod_data_source_block           Fe2Fe-290K
_cod_depositor_comments
'Adding full bibliography for 7707647--7707650.cif.'
_cod_database_code               7707649
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.931
_shelx_estimated_absorpt_t_min   0.889
_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. Shared sites
{C12A, N12}
3. Restrained distances
 O1-C32
 1.45 with sigma of 0.01
 O2_$1-H3A_$1
 1.6 with sigma of 0.01
4. Rigid bond restraints
 O1, C32
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
5. Uiso/Uaniso restraints and constraints
O1 \\sim C32: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C32) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O2) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C12A) = Uanis(N12)
Uanis(O2) = Uanis(O2A)
6. Others
 Sof(O2A)=Sof(H2AA)=Sof(H2AB)=0.5*(1-FVAR(2))
 Sof(O2)=Sof(H2A)=Sof(H2B)=0.5*FVAR(2)
 Fixed Sof: N12(0.5) H13A(0.5) H13(0.5) C12A(0.5) H12A(0.5) O1(0.5) H1B(0.5)
 C32(0.5) H32A(0.5) H32B(0.5) H32C(0.5) O3(0.5) H3A(0.5) H3B(0.5) O4(0.5)
 H4A(0.5) H4B(0.5)
7.a Riding coordinates:
 O1(H1B), C32(H32A,H32B,H32C), O2(H2A,H2B), O3(H3A,H3B), O4(H4A,H4B), O2A(H2AA,
 H2AB)
7.b Ternary CH refined with riding coordinates:
 B1(H1A)
7.c Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B)
7.d Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13A), C13(H13), C1(H1), C2(H2), C3(H3),
 C4(H4), C12A(H12A), C18(H18), C23(H23), C28(H28)
7.e Fitted hexagon refined as free rotating group:
 N12(C9,C10,C11,C12,C13)
7.f Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C)
;
_shelx_res_checksum              73073
_shelx_hkl_checksum              25266
_olex2_submission_special_instructions 'No special instructions were received'