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_7711317
_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 H90 B2 Co2 Fe2 N26 O4, 2(Cl O4), 3(C2 H3 N)'
_chemical_formula_sum            'C90 H99 B2 Cl2 Co2 Fe2 N29 O12'
_chemical_formula_weight         2101.06
_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             2022-09-05
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-09-05 deposited with the CCDC.	2022-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                81.971(5)
_cell_angle_beta                 73.964(5)
_cell_angle_gamma                79.688(6)
_cell_formula_units_Z            1
_cell_length_a                   12.017(2)
_cell_length_b                   14.179(2)
_cell_length_c                   15.527(3)
_cell_measurement_reflns_used    9860
_cell_measurement_temperature    103.68
_cell_measurement_theta_max      25.742
_cell_measurement_theta_min      2.470
_cell_volume                     2490.2(7)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      103.68
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_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  0.0574
_diffrn_reflns_av_unetI/netI     0.0811
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.970
_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       -16
_diffrn_reflns_number            17545
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.514
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.740
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.4977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1197 before and 0.0810 after correction. The Ratio of minimum to maximum transmission is 0.6678. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'dull dark green'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.863
_refine_diff_density_min         -0.867
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     661
_refine_ls_number_reflns         8507
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1472
_refine_ls_R_factor_gt           0.1053
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1065P)^2^+28.1388P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2474
_refine_ls_wR_factor_ref         0.2951
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5888
_reflns_number_total             8507
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02416k2.cif
_cod_data_source_block           100k1
_cod_database_code               7711317
_shelx_shelxl_version_number     2019/2
_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
2. Restrained distances
 C45-N15
 1.1 with sigma of 0.02
 C45-C46
 1.52 with sigma of 0.02
 C43-C44
 1.55 with sigma of 0.02
 N14-C43
 1.1 with sigma of 0.02
 N15-C46
 2.65 with sigma of 0.02
 O2B-C40
 1.4 with sigma of 0.02
 N14-C44
 2.65 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C45 \\sim C46 \\sim N15 \\sim N14 \\sim C43 \\sim C44: within 2A with sigma of
0.001 and sigma for terminal atoms of 0.02 within 2A
Uanis(N14) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(O2B)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: O2A(0.5) H2A(0.5) C43(0.5) C44(0.5) H44A(0.5) H44B(0.5) H44C(0.5)
 O2B(0.5) H2B(0.5) N14(0.5)
5.a Ternary CH refined with riding coordinates:
 B1(H1A)
5.b Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C30(H30A,H30B), C40(H40A,H40B)
5.c Aromatic/amide H refined with riding coordinates:
 C31(H31), C29(H29), C19(H19), C35(H35), C42(H42), C6(H6), C23(H23), C26(H26),
 C16(H16), C11(H11), C32(H32), C28(H28), C38(H38), C20(H20), C41(H41)
5.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C14(H14A,H14B,H14C), C9(H9A,H9B,H9C), C13(H13A,H13B,H13C),
 C8(H8A,H8B,H8C), C18(H18A,H18B,H18C), C22(H22A,H22B,H22C), C46(H46A,H46B,H46C),
  C44(H44A,H44B,H44C)
5.e Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2A(H2A), O2B(H2B)
;
_shelx_res_checksum              56145
_shelx_hkl_checksum              13926
_olex2_submission_special_instructions 'No special instructions were received'