Thermo- and photo-induced electron transfer in a series of [Fe<sub>2</sub>Co<sub>2</sub>] capsules.
Meng, Lingyi; Deng, Yi-Fei; Holmes, Stephen M.; Zhang, Yuan-Zhu; Dalton transactions (Cambridge, England : 2003) 52 (2023) 1616–1622; doi:10.1039/d2dt03328c

data_7712148
_publ_section_title
;
 Thermo- and photo-induced electron transfer in a series of
 [Fe<sub>2</sub>Co<sub>2</sub>] capsules.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1616
_journal_page_last               1622
_journal_paper_doi               10.1039/d2dt03328c
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety
'C104 H124 B2 Co2 Fe2 N30, 2(Cl O4), 4(C2 H3 N), C2 N'
_chemical_formula_sum            'C114 H136 B2 Cl2 Co2 Fe2 N35 O8'
_chemical_formula_weight         2446.65
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-06 deposited with the CCDC.	2022-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                72.318(5)
_cell_angle_beta                 73.993(5)
_cell_angle_gamma                69.773(5)
_cell_formula_units_Z            1
_cell_length_a                   14.246(2)
_cell_length_b                   15.814(2)
_cell_length_c                   16.329(2)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    260(2)
_cell_measurement_theta_max      26.401
_cell_measurement_theta_min      2.586
_cell_volume                     3228.2(7)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      260.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.985
_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  0.0588
_diffrn_reflns_av_unetI/netI     0.0476
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            53402
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.581
_diffrn_reflns_theta_min         2.231
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.580
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6116
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1281 before and 0.0633 after correction. The Ratio of minimum to maximum transmission is 0.8205. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       plate
_exptl_crystal_F_000             1279
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.969
_refine_diff_density_min         -0.699
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     778
_refine_ls_number_reflns         13284
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0574
_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^)+(0.1108P)^2^+2.4803P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1678
_refine_ls_wR_factor_ref         0.1927
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9704
_reflns_number_total             13284
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03328c2.cif
_cod_data_source_block           260k
_cod_depositor_comments
'Adding full bibliography for 7712143--7712148.cif.'
_cod_original_cell_volume        3228.3(8)
_cod_database_code               7712148
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.944
_shelx_estimated_absorpt_t_min   0.801
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  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
2. Restrained distances
 C58-N18B
 1.3 with sigma of 0.02
 C36-C35
 1.5 with sigma of 0.02
 C37-C36
 1.5 with sigma of 0.02
 C57B-C56
 1.5 with sigma of 0.02
 C56-N17B
 1.2 with sigma of 0.02
 C33-C34
 1.5 with sigma of 0.02
 C54-C55
 1.55 with sigma of 0.02
 C54-N16
 1.05 with sigma of 0.02
 N16-C55
 2.6 with sigma of 0.02
3. Rigid bond restraints
 C33, C32
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 H28
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim
C39A \\sim C39B \\sim C40 \\sim C41: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
H28: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.02
C55 \\sim C54 \\sim N16: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C33) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: N17B(0.5) C57A(0.5) H57A(0.5) H57B(0.5) H57C(0.5) H40A(0.5)
 H40B(0.5) H40C(0.5) H40D(0.5) C39B(0.5) H39A(0.5) H39B(0.5) H38A(0.5)
 H38B(0.5) H38C(0.5) H38D(0.5) C39A(0.5) H39C(0.5) H39D(0.5) C35(0.5) H35A(0.5)
 H35B(0.5) C57B(0.5) H57D(0.5) H57E(0.5) H57F(0.5) N17A(0.5) C34(0.5) H34A(0.5)
 H34B(0.5) N18A(0.25) N18B(0.25)
6.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B), C41(H41A,H41B), C40(H40A,H40B), C40(H40C,
 H40D), C37(H37A,H37B), C36(H36A,H36B), C39B(H39A,H39B), C38(H38A,H38B),
 C38(H38C,H38D), C39A(H39C,H39D), C35(H35A,H35B), C34(H34A,H34B), C33(H33A,H33B)
6.b Aromatic/amide H refined with riding coordinates:
 C43(H43), C20(H20), C19(H19), C49(H49), C26(H26), C53(H53), C52(H52),
 C44(H44), C16(H16), C29(H29), C23(H23), C28(H28), C46(H46), C6(H6), C11(H11),
 C30(H30), C42(H42)
6.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C4(H4A,H4B,H4C), C9(H9A,H9B,H9C), C18(H18A,H18B,H18C),
 C51(H51A,H51B,H51C), C8(H8A,H8B,H8C), C22(H22A,H22B,H22C), C13(H13A,H13B,H13C),
  C57A(H57A,H57B,H57C), C57B(H57D,H57E,H57F), C55(H55A,H55B,H55C)
;
_shelx_res_checksum              53650
_shelx_hkl_checksum              79423
_olex2_submission_special_instructions 'No special instructions were received'