Synthesis of triphenylene-fused phosphole oxides via C–H functionalizations
Rahman, Md Shafiqur; Yoshikai, Naohiko; Beilstein Journal of Organic Chemistry 16 (2020) 524–529; doi:10.3762/bjoc.16.48

data_4038140
_publ_section_title
;
 Synthesis of triphenylene-fused phosphole oxides via C--H
 functionalizations
;
_journal_name_full               'Beilstein Journal of Organic Chemistry'
_journal_page_first              524
_journal_page_last               529
_journal_paper_doi               10.3762/bjoc.16.48
_journal_volume                  16
_journal_year                    2020
_chemical_formula_sum            'C36 H37 O3 P'
_chemical_formula_weight         548.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90.8293(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.5972(2)
_cell_length_b                   23.8844(6)
_cell_length_c                   15.6911(3)
_cell_measurement_reflns_used    7947
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      28.2027
_cell_measurement_theta_min      2.5964
_cell_volume                     2846.92(12)
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_collection       'APEX3 (Bruker AXS Inc., 2016)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_molecular_graphics    'XP (Bruker AXS Inc., 2016)'
_computing_publication_material  'APEX3 (Bruker AXS Inc., 2016)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'XS, VERSION 2013/1'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 7.4074
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Photon II CPADs detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Multilayer Mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0725
_diffrn_reflns_av_unetI/netI     0.0599
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            36188
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.73
_diffrn_source                   'Incoatec microfocus source'
_diffrn_source_type              'Bruker D8 Quest'
_exptl_absorpt_coefficient_mu    0.133
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   'Numerical Mu Calculated'
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.221
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.154
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.372
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         7026
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0521
_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^)+(0.0324P)^2^+1.9886P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1011
_refine_ls_wR_factor_ref         0.1137
_reflns_number_gt                5336
_reflns_number_total             7026
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1860-5397-16-48-S2.cif
_cod_data_source_block           yoshi60m
_cod_depositor_comments          'Adding full bibliography for 4038140.cif.'
_cod_database_code               4038140
_shelx_res_checksum              8523
_shelx_hkl_checksum              76171