Peraryl-X-onium ions of nitrogen and oxygen
Lu, Mengsi; Allemann, Oliver; Xu, Jun; Linden, Anthony; Baldridge, Kim K.; Siegel, Jay S.; Organic Chemistry Frontiers 6 (2019) 2640–; doi:10.1039/C9QO00633H

data_1554984
_publ_section_title
;
 Peraryl-X-onium ions of nitrogen and oxygen
;
_journal_issue                   15
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              2640
_journal_paper_doi               10.1039/C9QO00633H
_journal_volume                  6
_journal_year                    2019
_chemical_formula_moiety         'C H6 B11 Cl6, C19 H15 O'
_chemical_formula_sum            'C20 H21 B11 Cl6 O'
_chemical_formula_weight         608.98
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-12 deposited with the CCDC.	2019-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.0146(6)
_cell_length_b                   13.8372(3)
_cell_length_c                   21.2518(5)
_cell_measurement_reflns_used    29092
_cell_measurement_temperature    113.15
_cell_measurement_theta_max      32.9370
_cell_measurement_theta_min      1.8940
_cell_volume                     5591.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      113.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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   -115.00  65.00   1.00    4.00    --  -25.00  45.00   0.00  180
  2  \w   -115.00  65.00   1.00    4.00    --  -25.00  45.00  90.00  180
  3  \w   -115.00  65.00   1.00    4.00    --  -25.00  45.00 180.00  180
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0025785000
_diffrn_orient_matrix_UB_12      0.0503279000
_diffrn_orient_matrix_UB_13      -0.0058893000
_diffrn_orient_matrix_UB_21      0.0208591000
_diffrn_orient_matrix_UB_22      0.0094895000
_diffrn_orient_matrix_UB_23      0.0269760000
_diffrn_orient_matrix_UB_31      0.0308142000
_diffrn_orient_matrix_UB_32      -0.0022410000
_diffrn_orient_matrix_UB_33      -0.0187491000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0511
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            49304
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         1.917
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.632
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82187
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_description       prism
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.444
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         4854
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0392
_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^)+(0.0542P)^2^+7.2759P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1062
_refine_ls_wR_factor_ref         0.1098
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4302
_reflns_number_total             4854
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9qo00633h2.cif
_cod_data_source_block           r20170322d_09302017
_cod_database_code               1554984
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H21 B11 Cl6 O'
_shelx_estimated_absorpt_t_max   0.884
_shelx_estimated_absorpt_t_min   0.884
_reflns_odcompleteness_completeness 98.38
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C14(H14), C15(H15), C12(H12), C18(H18), C17(H17), C5(H5), C11(H11),
 C10(H10), C2(H2), C3(H3), C4(H4)
2.b Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C)
2.c Boron cage BH refined with riding coordinates:
 B3(H3A), B2(H2A), B1(H1), B4(H4A), B5(H5A)
;
_shelx_res_checksum              11968
_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 1.188
_oxdiff_exptl_absorpt_empirical_full_min 0.846