A Convenient Method for the Preparation of N-Heterocyclic Bromophosphines: Excellent Precursors to the Corresponding N-Heterocyclic Phosphenium Salts
Dube, Jonathan W.; Farrar, Gregory J.; Norton, Erin L.; Szekely, Kara L. S.; Cooper, Benjamin F. T.; Macdonald, Charles L. B.; Organometallics 28 (2009) 4377–; doi:10.1021/om900420g

data_4069800
_publ_section_title
;
 A Convenient Method for the Preparation of N-Heterocyclic
 Bromophosphines: Excellent Precursors to the Corresponding N-Heterocyclic
 Phosphenium Salts
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4377
_journal_paper_doi               10.1021/om900420g
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C30 H28 Br N2 P'
_chemical_formula_weight         527.42
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.030(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   11.4785(12)
_cell_length_b                   17.6796(18)
_cell_length_c                   37.784(4)
_cell_measurement_reflns_used    5307
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.16
_cell_volume                     7657.0(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.3695
_diffrn_reflns_av_sigmaI/netI    0.3548
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            84740
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.08
_exptl_absorpt_coefficient_mu    1.694
_exptl_absorpt_correction_T_max  0.844
_exptl_absorpt_correction_T_min  0.691
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker 2001'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3264
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.544
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     919
_refine_ls_number_reflns         17321
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.3088
_refine_ls_R_factor_gt           0.1038
_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^)+(0.0784P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1603
_refine_ls_wR_factor_ref         0.2386
_reflns_number_gt                5437
_reflns_number_total             17321
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900420g_si_001.cif
_cod_data_source_block           p21c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        7657.1(14)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4069800