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_7152411
_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         'C21 H32 N P S Sn'
_chemical_formula_sum            'C21 H32 N P S Sn'
_chemical_formula_weight         480.2
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_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
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_audit_creation_date             2011-07-26T22:16:58-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 125.4060(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.62370(10)
_cell_length_b                   16.3773(2)
_cell_length_c                   15.8989(2)
_cell_measurement_reflns_used    10634
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.4261
_cell_measurement_theta_min      3.4078
_cell_volume                     2254.65(5)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_molecular_graphics    ORTEP-3
_computing_publication_material
;
WinGX Publication Routines
enCIFer
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Giacovazzo, 1992)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.264
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14406
_diffrn_reflns_theta_full        67.5
_diffrn_reflns_theta_max         68.55
_diffrn_reflns_theta_min         4.35
_exptl_absorpt_coefficient_mu    10.562
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.5559
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.931
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         4097
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0272
_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^)+(0.0407P)^2^+1.3175P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0686
_refine_ls_wR_factor_ref         0.0708
_reflns_number_gt                3813
_reflns_number_total             4097
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ob25395j.txt
_cod_data_source_block           newd
_cod_original_cell_volume        2254.65(4)
_cod_database_code               7152411