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_7709485
_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 H60 P2 Rh, C24 H12 B F40 S8'
_chemical_formula_sum            'C57 H72 B F40 P2 Rh S8'
_chemical_formula_weight         1949.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-12-03
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2021-12-07 deposited with the CCDC.	2022-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.572(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.4479(9)
_cell_length_b                   19.0194(10)
_cell_length_c                   20.1725(7)
_cell_measurement_reflns_used    3934
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      70.5910
_cell_measurement_theta_min      6.4750
_cell_volume                     7458.7(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -29.00  42.00   1.00   10.00    --    0.00  77.00 -90.00   71
  2  \w     44.00 126.00   1.00   20.00    --   54.00  38.00   0.00   82
  3  \w     27.00 108.00   1.00   20.00    --   54.00-125.00  90.00   81
  4  \w     46.00 100.00   1.00   20.00    --   54.00  57.00 -60.00   54
  5  \w     -9.00  73.00   1.00   20.00    --   54.00 -57.00 120.00   82
  6  \w     36.00 109.00   1.00   47.50    --  108.00-111.00-120.00   73
  7  \w     43.00 129.00   1.00   47.50    --  108.00 -38.00-120.00   86
  8  \w     38.00 109.00   1.00   47.50    --  108.00-111.00  60.00   71
  9  \w    105.00 174.00   1.00   47.50    --  108.00  77.00   0.00   69
 10  \w    116.00 178.00   1.00   47.50    --  108.00 111.00 -90.00   62
 11  \w     72.00 129.00   1.00   47.50    --  108.00 -63.00   0.00   57
 12  \w     46.00 119.00   1.00   47.50    --  108.00   0.00 -30.00   73
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0741325000
_diffrn_orient_matrix_UB_12      -0.0282353000
_diffrn_orient_matrix_UB_13      -0.0060204000
_diffrn_orient_matrix_UB_21      -0.0276156000
_diffrn_orient_matrix_UB_22      0.0758795000
_diffrn_orient_matrix_UB_23      -0.0020937000
_diffrn_orient_matrix_UB_31      0.0043861000
_diffrn_orient_matrix_UB_32      0.0000798000
_diffrn_orient_matrix_UB_33      -0.0761820000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_unetI/netI     0.0851
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            26754
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.928
_diffrn_reflns_theta_min         3.886
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.628
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.743
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.736
_exptl_crystal_description       block
_exptl_crystal_F_000             3928
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.112
_refine_diff_density_max         1.681
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     982
_refine_ls_number_reflns         13926
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1385
_refine_ls_R_factor_gt           0.0865
_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^)+(0.0936P)^2^+61.3202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2273
_refine_ls_wR_factor_ref         0.2587
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8569
_reflns_number_total             13926
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00335j2.cif
_cod_data_source_block           20133
_cod_database_code               7709485
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C57H72BF40P2RhS8
_chemical_oxdiff_usercomment     LD48H
_shelx_estimated_absorpt_t_max   0.571
_shelx_estimated_absorpt_t_min   0.528
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C10(H10), C16(H16), C22(H22), C28(H28), C3(H3), C6(H6)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B),
 C14(H14A,H14B), C15(H15A,H15B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B),
  C20(H20A,H20B), C21(H21A,H21B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,
 H25B), C26(H26A,H26B), C27(H27A,H27B), C29(H29A,H29B), C30(H30A,H30B),
 C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C1(H1A,H1B), C2(H2A,H2B),
 C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B)
2.c Aromatic/amide H refined with riding coordinates:
 C35(H35), C37(H37), C39(H39), C41(H41), C43(H43), C45(H45), C47(H47),
 C49(H49), C51(H51), C53(H53), C55(H55), C57(H57)
;
_shelx_res_checksum              62562
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.969
_oxdiff_exptl_absorpt_empirical_full_min 0.576