Synthesis of dihydrobenzazaphosphole ligands via an intramolecular cyclisation reaction
Leung, Wilson; Cosway, Sarah; Jones, Raymond H. V.; McCann, Hannah; Wills, Martin; Journal of the Chemical Society, Perkin Transactions 1  (2001) 2588–; doi:10.1039/b105495n

data_7204193
_publ_section_title
;
 Synthesis of dihydrobenzazaphosphole ligands via an intramolecular
 cyclisation reaction
;
_journal_issue                   20
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              2588
_journal_paper_doi               10.1039/b105495n
_journal_year                    2001
_chemical_formula_sum            'C18 H21 B Br N O P'
_chemical_formula_weight         389.05
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 96.7510(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   27.0233(2)
_cell_length_b                   14.3417(3)
_cell_length_c                   20.1259(4)
_cell_measurement_temperature    180(2)
_cell_volume                     7745.9(2)
_computing_structure_refinement  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_solution    'SHELXS-96 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_sigmaI/netI    0.1045
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19561
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.02
_exptl_absorpt_coefficient_mu    2.208
_exptl_absorpt_correction_T_max  0.8381
_exptl_absorpt_correction_T_min  0.5156
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_F_000             3184
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.043
_refine_diff_density_min         -0.927
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.018(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.947
_refine_ls_goodness_of_fit_obs   1.042
_refine_ls_matrix_type           full
_refine_ls_number_parameters     840
_refine_ls_number_reflns         13053
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      0.945
_refine_ls_restrained_S_obs      1.039
_refine_ls_R_factor_all          0.1126
_refine_ls_R_factor_obs          0.0521
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1167
_refine_ls_wR_factor_obs         0.0954
_reflns_number_observed          7522
_reflns_number_total             13053
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b105495n.txt
_cod_data_source_block           swb21
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      C2
_cod_database_code               7204193