[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_1542898
_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            'C27 H18 N3 O3 P'
_chemical_formula_weight         463.41
_chemical_name_common            YR6
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_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                89.311(2)
_cell_angle_beta                 88.175(2)
_cell_angle_gamma                67.8250(10)
_cell_formula_units_Z            4
_cell_length_a                   10.2381(6)
_cell_length_b                   13.0126(8)
_cell_length_c                   17.4162(11)
_cell_measurement_reflns_used    9874
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      34.3208
_cell_measurement_theta_min      2.1758
_cell_volume                     2147.6(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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'BRUKER APEX II CCD'
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0174
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            120588
_diffrn_reflns_theta_full        33.73
_diffrn_reflns_theta_max         33.73
_diffrn_reflns_theta_min         1.69
_diffrn_source                   'fine-focus tube'
_exptl_absorpt_coefficient_mu    0.165
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            'translucent intense red-green'
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'elongated prism'
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.610
_refine_diff_density_min         -0.291
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         17096
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+0.6492P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0979
_refine_ls_wR_factor_ref         0.1036
_reflns_number_gt                14842
_reflns_number_total             17096
_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.

2019-01-18
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum        'C54 H36 N6 O6 P2'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     926.83
_cod_database_code               1542898