Cluster dynamics of heterometallic trinuclear clusters during ligand substitution, redox chemistry, and group transfer processes.
Juda, Cristin E.; Handford, Rex C.; Bartholomew, Amymarie K.; Powers, Tamara M.; Gu, Nina X.; Meyer, Elisabeth; Roth, Nikolaj; Chen, Yu-Sheng; Zheng, Shao-Liang; Betley, Theodore A.; Chemical science 15 (2024) 8242–8248; doi:10.1039/d3sc03606e

data_1571006
_publ_section_title
;
 Cluster dynamics of heterometallic trinuclear clusters during ligand
 substitution, redox chemistry, and group transfer processes.
;
_journal_issue                   21
_journal_name_full               'Chemical science'
_journal_page_first              8242
_journal_page_last               8248
_journal_paper_doi               10.1039/d3sc03606e
_journal_volume                  15
_journal_year                    2024
_chemical_formula_sum            'C54 H88.5 Fe3 N7 O1.75 Si3'
_chemical_formula_weight         1115.63
_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   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-03-27 deposited with the CCDC.	2024-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.166(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4451(12)
_cell_length_b                   27.261(3)
_cell_length_c                   21.186(3)
_cell_measurement_reflns_used    9963
_cell_measurement_temperature    100
_cell_measurement_theta_max      14.9345
_cell_measurement_theta_min      2.2145
_cell_volume                     5897.1(13)
_computing_cell_refinement       'SAINT 8.35A (Bruker-AXS, 2015)'
_computing_data_collection       'APEX3 v2016.1.0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT 8.35A (Bruker-AXS, 2015)'
_computing_molecular_graphics    'Bruker SHELXTL (Sheldrick, 2015)'
_computing_publication_material  'Bruker SHELXTL (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
;
Bruker D8 goniometer with CCD area detector
;
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.1163
_diffrn_reflns_av_unetI/netI     0.0830
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            99679
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         14.997
_diffrn_reflns_theta_min         1.423
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.165
_exptl_absorpt_correction_T_max  0.7439
_exptl_absorpt_correction_T_min  0.6728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2382
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     745
_refine_ls_number_reflns         12080
_refine_ls_number_restraints     264
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0421
_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^)+2.2682P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1073
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9217
_reflns_number_total             12080
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc03606e2.cif
_cod_data_source_block           zsl
_cod_depositor_comments
'Adding full bibliography for 1571003--1571015.cif.'
_cod_original_cell_volume        5897.2(12)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C54 H88.50 Fe3 N7 O1.75 Si3'
_cod_database_code               1571006
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              90516