Planar Polycyclic Oxaphosphoranes Incorporating a Benzophosphole Unit.
Zhao, Xu; Gan, Zhenjie; Hu, Chaopeng; Duan, Zheng; Mathey, François; Organic letters 19 (2017) 5814–5817; doi:10.1021/acs.orglett.7b02769

data_1547676
_publ_section_title
;
 Planar Polycyclic Oxaphosphoranes Incorporating a Benzophosphole Unit.
;
_journal_issue                   21
_journal_name_full               'Organic letters'
_journal_page_first              5814
_journal_page_last               5817
_journal_paper_doi               10.1021/acs.orglett.7b02769
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety         'C26 H19 Cl P, Cl, H2 O'
_chemical_formula_sum            'C26 H21 Cl2 O P'
_chemical_formula_weight         451.30
_chemical_name_systematic
;
 ? 
;
_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_creation_date             2014-03-11
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                97.498(5)
_cell_angle_beta                 106.460(6)
_cell_angle_gamma                93.254(5)
_cell_formula_units_Z            2
_cell_length_a                   9.6822(6)
_cell_length_b                   10.6345(5)
_cell_length_c                   11.7489(8)
_cell_measurement_reflns_used    3587
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      71.9140
_cell_measurement_theta_min      3.9694
_cell_volume                     1144.63(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      291.15
_diffrn_detector_area_resol_mean 16.2312
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1612628000
_diffrn_orient_matrix_UB_12      -0.0227401000
_diffrn_orient_matrix_UB_13      0.0396873000
_diffrn_orient_matrix_UB_21      0.0381207000
_diffrn_orient_matrix_UB_22      0.1201621000
_diffrn_orient_matrix_UB_23      -0.0495878000
_diffrn_orient_matrix_UB_31      0.0184050000
_diffrn_orient_matrix_UB_32      0.0811213000
_diffrn_orient_matrix_UB_33      0.1228903000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15408
_diffrn_reflns_theta_full        67.10
_diffrn_reflns_theta_max         67.10
_diffrn_reflns_theta_min         3.97
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.323
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.23229
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour
;
;
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
;
_exptl_crystal_F_000             468
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.201
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         4094
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0728P)^2^+0.1032P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1189
_refine_ls_wR_factor_ref         0.1287
_reflns_number_gt                3262
_reflns_number_total             4094
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol7b02769_si_002.cif
_cod_data_source_block           20140334
_cod_depositor_comments
'Adding full bibliography for 1547674--1547677.cif.'
_cod_original_cell_volume        1144.62(12)
_cod_database_code               1547676
_chemical_oxdiff_formula         C20H20N4O4P1Cl2
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O1-H1B
 0.85 with sigma of 0.02
 O1-H1A
 0.85 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C22(H22), C23(H23), C24(H24),
  C25(H25), C26(H26)
;