Synthesis of Blue-Luminescent Seven-Membered Phosphorus Heterocycles
Regulska, Elzbieta; Ruppert, Heiko; Rominger, Frank; Romero-Nieto, Carlos; The Journal of Organic Chemistry  (2019) –; doi:10.1021/acs.joc.9b02723

data_4037702
_publ_section_title
;
 Synthesis of Blue-Luminescent Seven-Membered Phosphorus Heterocycles
;
_journal_name_full               'The Journal of Organic Chemistry'
_journal_paper_doi               10.1021/acs.joc.9b02723
_journal_year                    2019
_chemical_formula_sum            'C16 H18 B Br O2'
_chemical_formula_weight         333.02
_chemical_name_common            '3 in manuscript'
_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   geom
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
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_cell_length_b                   13.9012(5)
_cell_length_c                   16.9206(6)
_cell_measurement_reflns_used    3000
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      21.31
_cell_measurement_theta_min      2.41
_cell_volume                     3099.90(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
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_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II Quazar area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0643
_diffrn_reflns_av_unetI/netI     0.0540
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
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_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18649
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.033
_diffrn_reflns_theta_max         25.033
_diffrn_reflns_theta_min         2.407
_diffrn_source                   'ImuS microsource'
_exptl_absorpt_coefficient_mu    2.650
_exptl_absorpt_correction_T_max  0.8620
_exptl_absorpt_correction_T_min  0.7629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G. M. (2008). <i>SADABS</i>. University of G\"ottingen, Germany.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.813
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2743
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0555
_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^)+(0.0605P)^2^+7.5627P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1320
_refine_ls_wR_factor_ref         0.1491
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1928
_reflns_number_total             2743
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b02723_si_002.cif
_cod_data_source_block           crn28
_cod_database_code               4037702
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.836
_shelx_estimated_absorpt_t_max   0.836
_shelx_res_checksum              86873
_shelx_hkl_checksum              70542