MicroED characterization of a robust cationic σ-alkane complex stabilized by the [B(3,5-(SF5)2C6H3)4]− anion, via on-grid solid/gas single-crystal to single-crystal reactivity
Doyle, Laurence R.; Thompson, Emily A.; Burnage, Arron L.; Whitwood, Adrian C.; Jenkins, Huw T.; Macgregor, Stuart A.; Weller, Andrew S.; Dalton Transactions  (2022) –; doi:10.1039/D2DT00335J

data_7709481
_publ_section_title
;
 MicroED characterization of a robust cationic \s-alkane complex
 stabilized by the [B(3,5-(SF5)2C6H3)4]&#x2212; anion, via on-grid
 solid/gas single-crystal to single-crystal reactivity
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00335J
_journal_year                    2022
_chemical_formula_moiety         'C33 H56 P2 Rh, C24 H12 B F40 S8'
_chemical_formula_sum            'C57 H68 B F40 P2 Rh S8'
_chemical_formula_weight         1945.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-12-03 deposited with the CCDC.	2022-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.355(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.603(3)
_cell_length_b                   18.393(3)
_cell_length_c                   20.438(2)
_cell_measurement_reflns_used    982
_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      0.599
_cell_measurement_theta_min      0.064
_cell_volume                     7362.9(18)
_computing_cell_refinement       'DIALS (Winter et al., 2018)'
_computing_data_collection       EPU-D
_computing_data_reduction        'DIALS (Winter et al., 2018)'
_computing_molecular_graphics    'ShelXle (H\"ubschle et al., 2011)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      80(2)
_diffrn_detector                 CMOS
_diffrn_detector_area_resol_mean 35.7
_diffrn_detector_type            'Thermo Scientific Ceta-D'
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device       'electron microscope'
_diffrn_measurement_device_type  'Thermo Scientific Glacios'
_diffrn_measurement_method       'profile fitting from continuous rotation'
_diffrn_radiation_probe          electron
_diffrn_radiation_type           electron
_diffrn_radiation_wavelength     0.02508
_diffrn_reflns_av_R_equivalents  0.2348
_diffrn_reflns_av_unetI/netI     0.1680
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19560
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        0.758
_diffrn_reflns_theta_max         0.758
_diffrn_reflns_theta_min         0.063
_diffrn_source                   'electron microscope'
_diffrn_source_type              'Thermo Scientific Glacios'
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   'electron diffraction, unknown absorption'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_description       'nano crystals'
_exptl_crystal_F_000             1261
_exptl_crystal_size_max          0.0014
_exptl_crystal_size_mid          0.0005
_exptl_crystal_size_min          0.0001
_refine_diff_density_max         0.249
_refine_diff_density_min         -0.190
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       155(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.718
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         4380
_refine_ls_number_restraints     585
_refine_ls_restrained_S_all      1.633
_refine_ls_R_factor_all          0.2194
_refine_ls_R_factor_gt           0.1565
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3421
_refine_ls_wR_factor_ref         0.3584
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2563
_reflns_number_total             4380
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00335j2.cif
_cod_data_source_block           LD33E_g_b
_cod_original_cell_volume        7362.8(18)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7709481
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              70227