The crystal structure of 2,4,4-triphenyl-4H-benzo[b][1,4]oxaphosphinin-4-ium bromide – dichloromethane (1/1), C27H22BrCl2OP
Liu, Fen; Sun, Longgen; Huang, Haiyang; Zeitschrift für Kristallographie - New Crystal Structures 237 (2022) 509–511; doi:10.1515/ncrs-2022-0123

data_8105736
_publ_section_title
;
 The crystal structure of
 2,4,4-triphenyl-4H-benzo[b][1,4]oxaphosphinin-4-ium bromide --
 dichloromethane (1/1), C27H22BrCl2OP
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              509
_journal_page_last               511
_journal_paper_doi               10.1515/ncrs-2022-0123
_journal_volume                  237
_journal_year                    2022
_chemical_formula_moiety         'C26 H20 O P, C H2 Cl2, Br'
_chemical_formula_sum            'C27 H22 Br Cl2 O P'
_chemical_formula_weight         544.22
_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   geom
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 95.487(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0066(2)
_cell_length_b                   15.4924(4)
_cell_length_c                   18.5110(4)
_cell_measurement_reflns_used    4110
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.8300
_cell_measurement_theta_min      4.7890
_cell_volume                     2571.08(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2312
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega -106.00  -81.00   1.0000    1.2500
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  178.0000 -120.0000 25

  2 omega -102.00  -22.00   1.0000    1.2500
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -57.0000 -150.0000 80

  3 omega   10.00   44.00   1.0000    1.2500
omega____ theta____ kappa____ phi______ frames
    -       36.4734   77.0000   60.0000 34

  4 omega   60.00  108.00   1.0000    1.2500
omega____ theta____ kappa____ phi______ frames
    -       36.4734  178.0000  -90.0000 48

  5 omega   44.00   75.00   1.0000    1.2500
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -99.0000  -60.0000 31

  6 omega   55.00   94.00   1.0000    1.2500
omega____ theta____ kappa____ phi______ frames
    -       36.4734   77.0000   60.0000 39

  7 omega  -32.00   22.00   1.0000    1.2500
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -19.0000   90.0000 54

  8 omega   40.00   68.00   1.0000    1.2500
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -19.0000   90.0000 28

  9 omega    0.00   30.00   1.0000    1.2500
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -99.0000  -60.0000 30

 10 omega   80.00  106.00   1.0000    1.2500
omega____ theta____ kappa____ phi______ frames
    -       36.4734  178.0000    0.0000 26

 11 omega   57.00   85.00   1.0000    1.2500
omega____ theta____ kappa____ phi______ frames
    -       36.4734  178.0000 -180.0000 28

 12 omega   41.00   88.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -120.0000 47

 13 omega   96.00  144.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000  -30.0000 48

 14 omega   61.00   87.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -30.0000 26

 15 omega   40.00  102.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000   60.0000 62

 16 omega   42.00   95.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  -60.0000 53

 17 omega   37.00   62.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -180.0000 25

 18 omega   94.00  175.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000 -120.0000 81

 19 omega   73.00  111.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000    0.0000 38

 20 omega  110.00  175.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000    0.0000 65

 21 omega   41.00  115.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000   90.0000 74

 22 omega   39.00   65.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000    0.0000 26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0049311000
_diffrn_orient_matrix_UB_12      0.0899228000
_diffrn_orient_matrix_UB_13      -0.0352571000
_diffrn_orient_matrix_UB_21      0.0344364000
_diffrn_orient_matrix_UB_22      -0.0420129000
_diffrn_orient_matrix_UB_23      -0.0719534000
_diffrn_orient_matrix_UB_31      -0.1682413000
_diffrn_orient_matrix_UB_32      -0.0059800000
_diffrn_orient_matrix_UB_33      -0.0239642000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10289
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.071
_diffrn_reflns_theta_max         67.071
_diffrn_reflns_theta_min         3.728
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.808
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72523
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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    1.406
_exptl_crystal_description       prism
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.898
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4591
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0509
_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^)+(0.0862P)^2^+1.5448P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1399
_refine_ls_wR_factor_ref         0.1494
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3819
_reflns_number_total             4591
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0123_suppl.cif
_cod_data_source_block           2
_cod_original_cell_volume        2571.06(11)
_cod_database_code               8105736
_chemical_oxdiff_formula         C80H104O2N2P1Br1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C11(H11), C12(H12), C13(H13),
 C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23),
  C24(H24), C25(H25), C26(H26)
;
_olex2_submission_special_instructions 'No special instructions were received'