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_1554985
_publ_section_title
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 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, 2(C12 H8 N0.5)'
_chemical_formula_sum            'C25 H22 B11 Cl6 N'
_chemical_formula_weight         668.04
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-01-12
_audit_creation_method
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
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_audit_update_record
;
2019-01-12 deposited with the CCDC.	2019-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
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_cell_angle_gamma                90
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_cell_length_b                   18.4574(3)
_cell_length_c                   18.40020(17)
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_cell_measurement_temperature    160(2)
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_cell_measurement_theta_min      2.4640
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_computing_cell_refinement
'CrysAlisPro, Version 1.171.36.28 (Agilent Technologies, 2013)'
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'CrysAlisPro, Version 1.171.36.28 (Agilent Technologies, 2013)'
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'CrysAlisPro, Version 1.171.36.28 (Agilent Technologies, 2013)'
_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    'SHELXS-2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      160.15
_diffrn_detector_area_resol_mean 10.3801
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.860
_diffrn_measurement_device_type
'Oxford Diffraction SuperNova, dual radiation diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0209
_diffrn_reflns_av_unetI/netI     0.0190
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.860
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            39043
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.860
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.462
_diffrn_reflns_theta_min         2.207
_exptl_absorpt_coefficient_mu    0.562
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86616
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
CrysAlisPro, Version 1.171.36.28 (Agilent Technologies, 2013)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_description       prism
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         8322
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0307
_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^)+(0.0403P)^2^+2.4228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0833
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7016
_reflns_number_total             8322
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9qo00633h2.cif
_cod_data_source_block           sg1303
_cod_original_cell_volume        6352.02(13)
_cod_database_code               1554985
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8A), C9(H9A), C10(H10A), C11(H11A),
 C14(H14), C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C22(H22), C23(H23)
2.b Boron cage BH refined with riding coordinates:
 C25(H25), B7(H7), B8(H8), B9(H9), B10(H10), B11(H11)
;
_shelx_res_checksum              18541
_olex2_submission_special_instructions 'No special instructions were received'