Tuning the electron transfer events in a series of cyanide-bridged [Fe2Co2] squares according to different electron donors
Meng, Lingyi; Deng, Yi-Fei; Liu, Jianxun; Liu, Yan Jun; Zhang, Yuan-Zhu; Dalton Transactions  (2022) –; doi:10.1039/D2DT02416K

data_7711316
_publ_section_title
;
 Tuning the electron transfer events in a series of cyanide-bridged
 [Fe2Co2] squares according to different electron donors
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02416K
_journal_year                    2022
_chemical_formula_moiety
'C84 H84 B2 Co2 Fe2 N26 O4, 2(Cl O4), H2 O, C2 H3 N'
_chemical_formula_sum            'C86 H89 B2 Cl2 Co2 Fe2 N27 O13'
_chemical_formula_weight         2030.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-14 deposited with the CCDC.	2022-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.024(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9683(9)
_cell_length_b                   31.1073(17)
_cell_length_c                   22.8137(13)
_cell_measurement_reflns_used    9917
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.712
_cell_measurement_theta_min      2.264
_cell_volume                     9790.2(10)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_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  0.0932
_diffrn_reflns_av_unetI/netI     0.0897
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            89636
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.178
_diffrn_reflns_theta_min         2.245
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.750
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5418
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1078 before and 0.0633 after correction. The Ratio of minimum to maximum transmission is 0.7268. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'dull reddish red'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_description       block
_exptl_crystal_F_000             4192
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.637
_refine_diff_density_min         -1.628
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1221
_refine_ls_number_reflns         21663
_refine_ls_number_restraints     1743
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1382
_refine_ls_R_factor_gt           0.0909
_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^)+(0.1359P)^2^+34.9739P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2463
_refine_ls_wR_factor_ref         0.2789
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13611
_reflns_number_total             21663
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02416k2.cif
_cod_data_source_block           2
_cod_database_code               7711316
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.806
_shelx_estimated_absorpt_t_min   0.753
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C84-C83
 1.4 with sigma of 0.02
 N27_$1-O4
 3 with sigma of 0.02
3. Rigid bond restraints
 O4, C82, O1, C28, O2, C40, O3, C70
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.001
 C6, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C82, C81
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
O3 \\sim O4 \\sim O1 \\sim O2: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.02
O6A \\sim O8 \\sim O6B \\sim O9 \\sim O7: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
O2 \\sim C40 \\sim O1 \\sim C28 \\sim O4 \\sim C82: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
C66 \\sim C1 \\sim C2 \\sim C62 \\sim C43 \\sim C67 \\sim C47 \\sim C3 \\sim
C57 \\sim C44 \\sim C45 \\sim C61 \\sim C10 \\sim C36 \\sim C5 \\sim C52 \\sim
C78 \\sim C77 \\sim C37 \\sim C79 \\sim C58 \\sim C11 \\sim C25 \\sim C75 \\sim
C6 \\sim C59 \\sim C53 \\sim C72 \\sim C68 \\sim C56 \\sim C30 \\sim C9 \\sim
C0AA \\sim C4 \\sim C63 \\sim C46 \\sim C19 \\sim C51 \\sim C54 \\sim C48 \\sim
C71 \\sim C38 \\sim C73 \\sim C12 \\sim C24 \\sim C80 \\sim C65 \\sim C15 \\sim
C69 \\sim C60 \\sim C31 \\sim C39 \\sim C14 \\sim C49 \\sim C20 \\sim C55 \\sim
C1AA \\sim C29 \\sim C74 \\sim C81 \\sim C35 \\sim C21 \\sim C76 \\sim C70
\\sim C23 \\sim C50 \\sim C32 \\sim C17 \\sim C13 \\sim C41 \\sim C16 \\sim C42
\\sim C64 \\sim C26 \\sim C27 \\sim C33 \\sim C8 \\sim C82 \\sim C40 \\sim C18
\\sim C22 \\sim C34 \\sim C28 \\sim C83 \\sim C83 \\sim C84 \\sim C84: within
3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
O2 \\sim C40 \\sim O4 \\sim C82 \\sim O1 \\sim C28: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
C7 \\sim C6: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
O13 \\sim Cl2 \\sim O11 \\sim O10 \\sim O12 \\sim O8 \\sim Cl1 \\sim O9 \\sim
O6B \\sim O6A \\sim O7: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(O4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
5. Others
 Fixed Sof: O6B(0.5) O7(0.5)
6.a Free rotating group:
 O5(H5a,H5b)
6.b Ternary CH refined with riding coordinates:
 B1(H1), B2(H2)
6.c Aromatic/amide H refined with riding coordinates:
 C62(H62), C61(H61), C77(H77), C58(H58), C11(H11), C6(H6), C53(H53), C72(H72),
 C68(H68), C30(H30), C0AA(H0AA), C19(H19), C48(H48), C71(H71), C38(H38),
 C73(H73), C80(H80), C65(H65), C31(H31), C20(H20), C1AA(H1AA), C29(H29),
 C74(H74), C35(H35), C70(H70), C23(H23), C32(H32), C41(H41), C16(H16), C42(H42),
  C26(H26), C82(H82), C40(H40), C28(H28)
6.d Idealised Me refined as rotating group:
 C56(H56a,H56b,H56c), C9(H9a,H9b,H9c), C4(H4a,H4b,H4c), C46(H46a,H46b,H46c),
 C51(H51a,H51b,H51c), C60(H60a,H60b,H60c), C14(H14a,H14b,H14c), C55(H55a,H55b,
 H55c), C76(H76a,H76b,H76c), C50(H50a,H50b,H50c), C13(H13a,H13b,H13c), C64(H64a,
 H64b,H64c), C8(H8a,H8b,H8c), C18(H18a,H18b,H18c), C22(H22a,H22b,H22c),
 C34(H34a,H34b,H34c), C84(H84a,H84b,H84c)
;
_shelx_res_checksum              21689
_shelx_hkl_checksum              10403
_shelx_fab_checksum              71020
_olex2_submission_special_instructions 'No special instructions were received'