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_7707648
_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 Co Fe2 N23, 2(C H4 O), 2(H2 O)'
_chemical_formula_sum            'C65 H85 B2 Co Fe2 N23 O4'
_chemical_formula_weight         1444.80
_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             2019-08-06
_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                 111.544(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.763(2)
_cell_length_b                   22.329(2)
_cell_length_c                   15.4226(16)
_cell_measurement_reflns_used    6959
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.721
_cell_measurement_theta_min      2.651
_cell_volume                     7291.3(12)
_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      99.99
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0651
_diffrn_reflns_av_unetI/netI     0.0561
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23502
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        24.780
_diffrn_reflns_theta_max         24.780
_diffrn_reflns_theta_min         2.185
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.679
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.5952
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1088 before and 0.0634 after correction. The Ratio of minimum to maximum transmission is 0.7988. 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    1.316
_exptl_crystal_description       block
_exptl_crystal_F_000             3028
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.408
_refine_diff_density_min         -1.055
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         6219
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1115
_refine_ls_R_factor_gt           0.0860
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1760P)^2^+43.5018P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2644
_refine_ls_wR_factor_ref         0.2929
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4529
_reflns_number_total             6219
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01298c3.cif
_cod_data_source_block           Fe2Co-100K
_cod_depositor_comments
'Adding full bibliography for 7707647--7707650.cif.'
_cod_database_code               7707648
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.887
_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
{N12, C1A}
3. Restrained distances
 N2-C8
 1.5 with sigma of 0.001
 H2-H32A
 2 with sigma of 0.01
 H33A-H30C
 2 with sigma of 0.01
 O1-C32 = O2-C33
 1.45 with sigma of 0.01
4. Rigid bond restraints
 N12, C9, C10, C11, C12, C13
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 N2, C7
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 N2, C8
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 O1, C32
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 O2, C33
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
5. Uiso/Uaniso restraints and constraints
N12 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04
N2 \\sim C7: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
N2 \\sim C8: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
O1 \\sim C32: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
O2 \\sim C33: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(N12) = Uanis(C1A)
6. Others
 Fixed Sof: O1(0.5) H1C(0.5) O2(0.5) H2A(0.5) O4(0.5) H4A(0.5) H4B(0.5)
 O5(0.5) H5A(0.5) H5B(0.5) C1A(0.5) H1A(0.5) H13(0.5) H13A(0.5) N12(0.5)
 C32(0.5) H32A(0.5) H32B(0.5) H32C(0.5) C33(0.5) H33A(0.5) H33B(0.5) H33C(0.5)
7.a Riding coordinates:
 O1(H1C), O2(H2A), O4(H4A,H4B), O5(H5A,H5B), C33(H33A,H33B,H33C)
7.b Ternary CH refined with riding coordinates:
 B1(H1B)
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:
 C1(H1), C1A(H1A), C2(H2), C3(H3), C4(H4), C13(H13), C13(H13A), C12(H12),
 C11(H11), C10(H10), C18(H18), C23(H23), C28(H28)
7.e Fitted hexagon refined as free rotating group:
 C13(C12,C11,C10,C9,N12)
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), C32(H32A,H32B,H32C)
;
_shelx_res_checksum              21735
_shelx_hkl_checksum              39118
_olex2_submission_special_instructions 'No special instructions were received'