Synthetic, structural, NMR and catalytic studies of phosphinic amide-phosphoryl chalcogenides (chalcogen = O, S, Se) as mixed-donor bidentate ligands in zinc chemistry.
Del Águila-Sánchez, Miguel A; Santos-Bastos, Neidemar M; Ramalho-Freitas, Maria C; García López, Jesús; Costa de Souza, Marcos; Camargos-Resende, Jackson A L; Casimiro, María; Alves-Romeiro, Gilberto; Iglesias, María José; López Ortiz, Fernando; Dalton transactions (Cambridge, England : 2003) 43 (2014) 14079–14091; doi:10.1039/c4dt01789g

data_7032456
_publ_section_title
;
 Synthetic, structural, NMR and catalytic studies of phosphinic
 amide-phosphoryl chalcogenides (chalcogen = O, S, Se) as mixed-donor
 bidentate ligands in zinc chemistry.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14079
_journal_page_last               14091
_journal_paper_doi               10.1039/c4dt01789g
_journal_volume                  43
_journal_year                    2014
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C30 H33 N O P2 S, C2 H3 N'
_chemical_formula_sum            'C32 H36 N2 O P2 S'
_chemical_formula_weight         558.63
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-01-09T00:36:00-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                93.263(18)
_cell_angle_beta                 94.429(17)
_cell_angle_gamma                109.92(2)
_cell_formula_units_Z            2
_cell_length_a                   9.1412(13)
_cell_length_b                   9.8502(17)
_cell_length_c                   17.910(4)
_cell_measurement_reflns_used    10898
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      3.5
_cell_measurement_wavelength     0.71073
_cell_volume                     1505.7(5)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2006)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10185
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         3.519
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.241
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS; Sheldrick, 1996
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.129
_exptl_crystal_size_min          0.095
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         5486
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.927
_refine_ls_R_factor_all          0.1062
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0415P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.1112
_reflns_number_gt                3173
_reflns_number_total             5486
_reflns_threshold_expression     'I > 2\s(I)'
_cod_duplicate_entry             7031812
_cod_data_source_file            c4dt01789g2.cif
_cod_data_source_block           n172
_cod_original_cell_volume        1505.6(5)
_cod_database_code               7032456