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_7711318
_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 H92 B2 Co2 Fe2 N26 O8, 2(Cl O4), 4(C O)'
_chemical_formula_sum            'C88 H92 B2 Cl2 Co2 Fe2 N26 O20'
_chemical_formula_weight         2155.95
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-20
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2021-12-01 deposited with the CCDC.	2022-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                85.221(3)
_cell_angle_beta                 74.071(3)
_cell_angle_gamma                79.083(2)
_cell_formula_units_Z            1
_cell_length_a                   11.8997(8)
_cell_length_b                   14.1917(11)
_cell_length_c                   15.8456(12)
_cell_measurement_reflns_used    7587
_cell_measurement_temperature    109.99
_cell_measurement_theta_max      26.396
_cell_measurement_theta_min      2.517
_cell_volume                     2525.2(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      109.99
_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  0.0707
_diffrn_reflns_av_unetI/netI     0.1062
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20311
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         2.515
_diffrn_source_current           1.2
_diffrn_source_power             0.0576
_diffrn_source_voltage           48.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.736
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1388 before and 0.0846 after correction.
The Ratio of minimum to maximum transmission is 0.7769.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_description       block
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.880
_refine_diff_density_min         -1.241
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     659
_refine_ls_number_reflns         8847
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1316
_refine_ls_R_factor_gt           0.0911
_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^)+(0.1600P)^2^+8.1943P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2523
_refine_ls_wR_factor_ref         0.2870
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5796
_reflns_number_total             8847
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02416k2.cif
_cod_data_source_block           3
_cod_database_code               7711318
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.867
_shelx_estimated_absorpt_t_min   0.710
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C43-O9
 1.5 with sigma of 0.02
 H2_$1-H3_$2
 2.1 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O10 \\sim C44 \\sim C43 \\sim O9: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
4. Others
 Fixed Sof: H40a(0.5) H40b(0.5) H40c(0.5) H40d(0.5) O4B(0.5) H4Ba(0.5)
 O4A(0.5) H4Aa(0.5) O8B(0.5) O8A(0.5)
5.a Ternary CH refined with riding coordinates:
 B1(H1a)
5.b Secondary CH2 refined with riding coordinates:
 C22(H22a,H22b), C28(H28a,H28b), C40(H40a,H40b), C40(H40c,H40d), C34(H34a,H34b)
5.c Aromatic/amide H refined with riding coordinates:
 C23(H23), C26(H26), C42(H42), C19(H19), C20(H20), C30(H30), C31(H31),
 C29(H29), C38(H38), C41(H41), C32(H32), C6(H6), C35(H35), C16(H16), C11(H11)
5.d Idealised Me refined as rotating group:
 C4(H4a,H4b,H4c), C9(H9a,H9b,H9c), C8(H8a,H8b,H8c), C14(H14a,H14b,H14c),
 C18(H18a,H18b,H18c), C13(H13a,H13b,H13c)
5.e Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2), O3(H3), O4B(H4Ba), O4A(H4Aa)
;
_shelx_res_checksum              33091
_shelx_hkl_checksum              49403
_olex2_submission_special_instructions 'No special instructions were received'