Transformations of diphenylphosphinothioic acid tertiary amides mediated by directed ortho metallation.
El Hajjouji, Hajar; Belmonte, Eva; García-López, Jesús; Fernández, Ignacio; Iglesias, María José; Roces, Laura; García-Granda, Santiago; El Laghdach, Anas; López Ortiz, Fernando; Organic & biomolecular chemistry 10 (2012) 5647–5658; doi:10.1039/c2ob25395j

data_7152410
_publ_section_title
;
 Transformations of diphenylphosphinothioic acid tertiary amides mediated
 by directed ortho metallation.
;
_journal_issue                   29
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              5647
_journal_page_last               5658
_journal_paper_doi               10.1039/c2ob25395j
_journal_volume                  10
_journal_year                    2012
_chemical_formula_moiety         'C30 H33 N P2 S'
_chemical_formula_sum            'C30 H33 N P2 S'
_chemical_formula_weight         501.57
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2011-10-02T19:17:14-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 119.548(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6300(5)
_cell_length_b                   10.2681(3)
_cell_length_c                   22.3237(6)
_cell_measurement_reflns_used    9585
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.41
_cell_measurement_theta_min      2.49
_cell_volume                     2717.96(16)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material
;
WinGX Publication Routines
enCIFer
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0906
_diffrn_reflns_av_unetI/netI     0.0585
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            13903
_diffrn_reflns_theta_full        24.42
_diffrn_reflns_theta_max         24.42
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.256
_exptl_absorpt_correction_T_max  1.0473
_exptl_absorpt_correction_T_min  0.6756
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56
Linear fit to sin(theta)/lambda - 12 parameters
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          1.41
_exptl_crystal_size_mid          0.429
_exptl_crystal_size_min          0.339
_refine_diff_density_max         0.62
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         4468
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0518P)^2^+1.6859P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.108
_refine_ls_wR_factor_ref         0.1095
_reflns_number_gt                4164
_reflns_number_total             4468
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ob25395j.txt
_cod_data_source_block           MAS
_cod_original_cell_volume        2717.96(15)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7152410