Tailoring Buchwald-Type Phosphines with Pyrimidinium Betaines as Versatile Aryl Group Surrogates
Noël-Duchesneau, Ludovik; Lugan, Noël; Lavigne, Guy; Labande, Agnès; César, Vincent; Organometallics 33 (2014) 5085–; doi:10.1021/om5007819

data_4084343
_publ_section_title
;
 Tailoring Buchwald-Type Phosphines with Pyrimidinium Betaines as
 Versatile Aryl Group Surrogates
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5085
_journal_paper_doi               10.1021/om5007819
_journal_volume                  33
_journal_year                    2014
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C29 H31 N2 O2 P'
_chemical_formula_sum            'C29 H31 N2 O2 P'
_chemical_formula_weight         470.53
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-01-23T10:16:08-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.7435(5)
_cell_length_b                   13.1941(3)
_cell_length_c                   9.6988(3)
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      31.2355
_cell_measurement_theta_min      3.2493
_cell_volume                     2526.52(12)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
        (compiled May 29 2009,17:40:42)
;
_computing_data_collection
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        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
        (compiled May 29 2009,17:40:42)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
        (compiled May 29 2009,17:40:42)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.1978
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0307112000
_diffrn_orient_matrix_UB_12      0.0267232000
_diffrn_orient_matrix_UB_13      -0.0110259000
_diffrn_orient_matrix_UB_21      0.0178784000
_diffrn_orient_matrix_UB_22      -0.0465925000
_diffrn_orient_matrix_UB_23      -0.0026120000
_diffrn_orient_matrix_UB_31      -0.0053221000
_diffrn_orient_matrix_UB_32      -0.0024141000
_diffrn_orient_matrix_UB_33      -0.0722276000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_unetI/netI     0.0114
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            37005
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.26
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.137
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
        (compiled May 29 2009,17:40:42)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.223
_refine_diff_density_min         -0.16
_refine_diff_density_rms         0.029
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         5152
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.026
_refine_ls_R_factor_gt           0.0253
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0434P)^2^+0.4696P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.068
_refine_ls_wR_factor_ref         0.0688
_reflns_number_gt                5053
_reflns_number_total             5152
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om5007819_si_002.cif
_cod_data_source_block           compound_4a
_cod_depositor_comments
'Adding full bibliography for 4084343--4084346.cif.'
_cod_database_code               4084343