[d]-Carbon‒carbon double bond engineering in diazaphosphepines: a pathway to modulate the chemical and electronic structures of heteropines
Ren, Yi; Sezen, Melda; Guo, Fang; Jäkle, Frieder; Loo, Yueh-Lin; Chem. Sci. 7 (2016) 4211–; doi:10.1039/C6SC00519E

data_1542894
_publ_section_title
;
 [d]-Carbon--carbon double bond engineering in diazaphosphepines: a
 pathway to modulate the chemical and electronic structures of heteropines
;
_journal_issue                   7
_journal_name_full               'Chem. Sci.'
_journal_page_first              4211
_journal_paper_doi               10.1039/C6SC00519E
_journal_volume                  7
_journal_year                    2016
_chemical_formula_sum            'C17 H10.5 N P0.5'
_chemical_formula_weight         244.25
_chemical_name_common            YR1
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2015-09-25 deposited with the CCDC.
2016-03-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.8239(8)
_cell_length_b                   19.3822(10)
_cell_length_c                   7.8312(4)
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      33.7105
_cell_measurement_theta_min      2.5745
_cell_volume                     2401.8(2)
_computing_cell_refinement       'SAINT V8.30C (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker Instrument Service v2012.12.0.3'
_computing_data_reduction        'SAINT V8.30C (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'BRUKER APEX II CCD'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            52792
_diffrn_reflns_theta_full        36.37
_diffrn_reflns_theta_max         36.37
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    0.142
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            'translucent intense red-purple'
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular rhombic shard'
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.664
_refine_diff_density_min         -0.439
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.912
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         5933
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      0.944
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0598P)^2^+2.2881P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1197
_refine_ls_wR_factor_ref         0.1312
_reflns_number_gt                4817
_reflns_number_total             5933
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6sc00519e2.cif
_cod_data_source_block           I
_cod_depositor_comments
'Adding full bibliography for 1542894--1542898.cif.'
_cod_original_formula_sum        'C17 H10.50 N P0.50'
_cod_database_code               1542894