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_1554987
_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         'C24 H18 N, C H6 B11 Cl6'
_chemical_formula_sum            'C25 H24 B11 Cl6 N'
_chemical_formula_weight         670.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-12-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-16 deposited with the CCDC.	2019-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.6660(10)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   31.445(2)
_cell_length_b                   13.6072(8)
_cell_length_c                   32.634(2)
_cell_measurement_reflns_used    16297
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     12478.2(13)
_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 (Sheldrick, 2008)'
_diffrn_ambient_temperature      113
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rigaku Xtalab P200'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0727
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            124044
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.549
_diffrn_reflns_theta_min         2.994
_exptl_absorpt_coefficient_mu    0.572
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   REQAB(Rigaku,1998)
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             5408
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.452
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1565
_refine_ls_number_reflns         28478
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.1074
_refine_ls_R_factor_gt           0.0711
_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^)+(0.0241P)^2^+39.1817P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1348
_refine_ls_wR_factor_ref         0.1534
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21156
_reflns_number_total             28478
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9qo00633h2.cif
_cod_data_source_block           diarylammonium
_cod_original_cell_volume        12478.3(15)
_cod_database_code               1554987
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.914
_shelx_estimated_absorpt_t_min   0.884
_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:
 C6(H6), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13), C14(H14), C15(H15),
 C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25), C26(H26),
  C27(H27), C28(H28), C30(H30), C31(H31), C32(H32), C33(H33), C36(H36),
 C37(H37), C38(H38), C39(H39), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46),
  C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C54(H54), C55(H55),
 C56(H56), C57(H57), C60(H60), C61(H61), C62(H62), C63(H63), C66(H66), C67(H67),
  C68(H68), C69(H69), C70(H70), C72(H72), C73(H73), C74(H74), C75(H75),
 C76(H76), C78(H78), C79(H79), C80(H80), C81(H81), C84(H84), C85(H85), C86(H86),
  C87(H87), C90(H90), C91(H91), C92(H92), C93(H93), C94(H94), C96(H96),
 C97(H97), C98(H98), C99(H99), C100(H100)
2.b Boron cage BH refined with riding coordinates:
 B7(H7A), B8(H8A), B9(H9A), B10(H10), B11(H11), B18(H18A), B19(H19A),
 B20(H20A), B21(H21A), B22(H22A), B29(H29), B30(H30A), B31(H31A), B32(H32A),
 B33(H33A), B40(H40), B41(H41), B42(H42A), B43(H43A), B44(H44A)
;
_shelx_res_checksum              71907
_olex2_submission_special_instructions 'No special instructions were received'