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_7709484
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-05-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-12-07 deposited with the CCDC.	2022-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.460(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.5793(9)
_cell_length_b                   18.3333(6)
_cell_length_c                   20.4528(7)
_cell_measurement_reflns_used    3029
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      70.8500
_cell_measurement_theta_min      6.8820
_cell_volume                     7334.8(5)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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 0.996
_diffrn_measured_fraction_theta_max 0.974
_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    -44.00  -8.00   1.00   10.00    --    0.00 125.00 -39.00   36
  2  \w    -20.00  22.00   1.00   10.00    --    0.00 -77.00-120.00   42
  3  \w     -4.00  29.00   1.00   10.00    --    0.00 -77.00  90.00   33
  4  \w     39.00  71.00   1.00   40.00    --   54.00 -57.00-120.00   32
  5  \w     50.00 104.00   1.00   40.00    --   54.00-125.00 120.00   54
  6  \w      6.00  75.00   1.00   40.00    --   54.00 -38.00  90.00   69
  7  \w    -15.00  50.00   1.00   40.00    --   54.00 -57.00   0.00   65
  8  \w     55.00 121.00   1.00   40.00    --   54.00  59.00  86.00   66
  9  \w    111.00 171.00   1.00   60.00    --  108.00  77.00  30.00   60
 10  \w    126.00 172.00   1.00   60.00    --  108.00  77.00 -60.00   46
 11  \w     36.00  67.00   1.00   60.00    --  108.00 -91.00-150.00   31
 12  \w    132.00 174.00   1.00   60.00    --  108.00  50.00 -30.00   42
 13  \w     37.00 130.00   1.00   60.00    --  108.00 -38.00 -60.00   93
 14  \w    123.00 149.00   1.00   60.00    --  108.00 111.00  90.00   26
 15  \w    103.00 177.00   1.00   60.00    --  108.00  77.00   0.00   74
 16  \w     83.00 175.00   1.00   60.00    --  108.00  38.00 120.00   92
;
_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      -0.0569449000
_diffrn_orient_matrix_UB_12      -0.0558643000
_diffrn_orient_matrix_UB_13      -0.0162198000
_diffrn_orient_matrix_UB_21      -0.0047400000
_diffrn_orient_matrix_UB_22      -0.0171952000
_diffrn_orient_matrix_UB_23      0.0734553000
_diffrn_orient_matrix_UB_31      -0.0542205000
_diffrn_orient_matrix_UB_32      0.0602528000
_diffrn_orient_matrix_UB_33      0.0058794000
_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  0.0554
_diffrn_reflns_av_unetI/netI     0.0880
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13332
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.091
_diffrn_reflns_theta_min         3.896
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.723
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.908
_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    1.762
_exptl_crystal_description       block
_exptl_crystal_F_000             3912
_exptl_crystal_size_max          0.071
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.041
_refine_diff_density_max         1.361
_refine_diff_density_min         -1.137
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         6921
_refine_ls_number_restraints     402
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1024
_refine_ls_R_factor_gt           0.0660
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0807P)^2^+46.0846P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1627
_refine_ls_wR_factor_ref         0.1834
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4790
_reflns_number_total             6921
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00335j2.cif
_cod_data_source_block           asw21048
_cod_database_code               7709484
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C57H68BF40P2RhS8
_chemical_oxdiff_usercomment     LD33E
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 S2-F10 \\sim S3-F15 \\sim S4-F20 \\sim S1A-F5A \\sim S1-F5
 with sigma of 0.02
 S1-C20 \\sim S1A-C20 \\sim S2-C22 \\sim S4-C28 \\sim S3-C26
 with sigma of 0.02
 S2-F7 \\sim S2-F6 \\sim S2-F9 \\sim S2-F8 \\sim S3-F12 \\sim S3-F13 \\sim
S3-F14 \\sim S3-F11 \\sim S4-F18 ~
 S4-F17 \\sim S4-F16 \\sim S4-F19 \\sim S1-F3 \\sim S1-F4 \\sim S1-F1 \\sim
S1-F2 \\sim S1A-F3A \\sim S1A-F4A ~
 S1A-F1A \\sim S1A-F2A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
S1 \\sim S1A \\sim F1 \\sim F1A \\sim F2 \\sim F2A \\sim F3 \\sim F3A \\sim F4
\\sim F4A \\sim F5 \\sim F5A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
4. Others
 Sof(S1A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=1-FVAR(1)
 Sof(S1)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=FVAR(1)
 Fixed Sof: H4A(0.5) H4B(0.5)
5.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C12(H12)
5.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,
 H10B), C11(H11A,H11B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B),
 C16(H16A,H16B), C17(H17A,H17B)
5.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C21(H21), C23(H23), C25(H25), C27(H27), C29(H29)
;
_shelx_res_checksum              95927
_olex2_date_sample_data_collection 2021-04-12
_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 2.289
_oxdiff_exptl_absorpt_empirical_full_min 0.694