Stereoselective addition of diphenylphosphine to substituted diphenylethynes: synthetic, NMR and X-ray crystallographic studies
Bookham, Jonathan L.; Smithies, Darren M.; Wright, Anna; Thornton-Pett, Mark; McFarlane, William; Journal of the Chemical Society, Dalton Transactions  (1998) 811–; doi:10.1039/a707210d

data_7027980
_publ_section_title
;
 Stereoselective addition of diphenylphosphine to substituted
 diphenylethynes: synthetic, NMR and X-ray crystallographic studies
;
_journal_issue                   5
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              811
_journal_paper_doi               10.1039/a707210d
_journal_year                    1998
_chemical_formula_sum            'C26 H21 P'
_chemical_formula_weight         364.40
_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_date             97-07-18
_audit_creation_method           'STADI4, X-RED'
_cell_angle_alpha                90.00
_cell_angle_beta                 100.484(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.2602(6)
_cell_length_b                   6.0689(3)
_cell_length_c                   27.289(2)
_cell_measurement_reflns_used    80
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      40.0
_cell_measurement_theta_min      35.0
_cell_volume                     1996.6(2)
_computing_cell_refinement       'DIF4 (STOE, 1989)'
_computing_data_collection       'DIF4 (STOE, 1989)'
_computing_data_reduction        'X-RED  (STOE, 1996)'
_computing_molecular_graphics    'ORTEX (McArdle, 1996)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'STOE STADI4 4-circle-diffractometer'
_diffrn_measurement_method
;
   Scan width (omega) = 1.23 - 1.50, scan ratio 2theta:omega = 1.00
;
_diffrn_radiation_collimation    '0.8 mm'
_diffrn_radiation_detector       'NaI(Tl) scintillation counter'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_polarisn_norm  90
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0192
_diffrn_reflns_av_sigmaI/netI    0.0219
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            6513
_diffrn_reflns_theta_full        64.61
_diffrn_reflns_theta_max         64.61
_diffrn_reflns_theta_min         3.29
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.248
_exptl_absorpt_correction_T_max  0.7884
_exptl_absorpt_correction_T_min  0.6222
_exptl_absorpt_process_details
;
    Psi Scan Reflections used    Mu * R = 0.02  

    H   K   L   2Theta   Chi   Imin/Imax
    1   3   0    45.5   -84.2    0.910
   -1  -3   0    45.5    84.2    0.904
    2   6   0   101.2   -84.2    0.913
   -2  -6   0   101.2    84.2    0.852
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.161
_refine_diff_density_min         -0.149
_refine_diff_density_rms         0.027
_refine_ls_extinction_coef       0.0060(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3297
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+0.4537P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0874
_reflns_number_gt                2800
_reflns_number_total             3297
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d707210sup1.cif
_cod_data_source_block           JLB3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+0.4537P] 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^)+(0.0397P)^2^+0.4537P] 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      P21/c
_cod_database_code               7027980
_audit_contact_author            'J. Richter'