Self-assembly of an organometallic Fe<sub>9</sub>O<sub>6</sub> cluster from aerobic oxidation of (tmeda)Fe(CH<sub>2</sub><sup>t</sup>Bu)<sub>2</sub>.
Kephart, Jonathan A.; Hecht, Zachary; Livesay, Brooke N.; Bhowmick, Indrani; Shores, Matthew P.; Popescu, V. Codrina; Arulsamy, Navamoney; Hulley, Elliott B.; Chemical communications (Cambridge, England) 56 (2020) 4994–4997; doi:10.1039/d0cc00011f

data_7126211
_publ_section_title
;
 Self-assembly of an organometallic Fe<sub>9</sub>O<sub>6</sub> cluster
 from aerobic oxidation of
 (tmeda)Fe(CH<sub>2</sub><sup>t</sup>Bu)<sub>2</sub>.
;
_journal_issue                   37
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4994
_journal_page_last               4997
_journal_paper_doi               10.1039/d0cc00011f
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C48 H114 Fe9 N6 O6, C5 H12'
_chemical_formula_sum            'C53 H126 Fe9 N6 O6'
_chemical_formula_weight         1446.24
_space_group_crystal_system      trigonal
_space_group_IT_number           155
_space_group_name_Hall           'R 3 2"'
_space_group_name_H-M_alt        'R 3 2 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2020-01-01 deposited with the CCDC.	2020-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   16.9429(13)
_cell_length_b                   16.9429(13)
_cell_length_c                   23.233(2)
_cell_measurement_reflns_used    7583
_cell_measurement_temperature    116(2)
_cell_measurement_theta_max      28.97
_cell_measurement_theta_min      2.41
_cell_volume                     5775.8(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      116(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.992
_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  0.0427
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            28320
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.123
_diffrn_reflns_theta_min         3.564
_exptl_absorpt_coefficient_mu    1.683
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6716
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SAINT'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_description       parallelpiped
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_platon_squeeze_details
; 
The SQUEEZE/PLATON program was used to remvoe scattering due to 
the three highly disordered n-pentane molecules in the unit cell. 
;
_refine_diff_density_max         0.267
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details
; 
 Flack x determined using 1650 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.001(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     105
_refine_ls_number_reflns         4860
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0211P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0483
_refine_ls_wR_factor_ref         0.0519
_reflns_Friedel_coverage         0.837
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                4068
_reflns_number_total             4860
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc00011f2.cif
_cod_data_source_block           jk15_sq
_cod_depositor_comments
'Adding full bibliography for 7126210--7126211.cif.'
_cod_original_cell_volume        5775.8(12)
_cod_original_sg_symbol_Hall     'R 3 2"''
_cod_original_sg_symbol_H-M      'R 3 2 :h'
_cod_database_code               7126211
_shelx_shelxl_version_number     2016/6
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              20678
_shelx_fab_checksum              82298