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_7032457
_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 Cl2 N1 O2 P2 Zn1'
_chemical_formula_sum            'C30 H33 Cl2 N O2 P2 Zn'
_chemical_formula_weight         637.78
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_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
_audit_creation_date             2013-12-10T22:51:09-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 91.666(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7651(4)
_cell_length_b                   15.5932(5)
_cell_length_c                   17.9816(6)
_cell_measurement_reflns_used    3769
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.4913
_cell_measurement_theta_min      1.8887
_cell_measurement_wavelength     0.71073
_cell_volume                     3017.16(18)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
        (compiled Aug  3 2011,13:03:54)
;
_computing_data_collection
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
        (compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
        (compiled Aug  3 2011,13:03:54)
;
_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_area_resol_mean 10.4186
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0547252
_diffrn_orient_matrix_UB_12      0.025377
_diffrn_orient_matrix_UB_13      -0.0002164
_diffrn_orient_matrix_UB_21      0.0165074
_diffrn_orient_matrix_UB_22      0.0182532
_diffrn_orient_matrix_UB_23      -0.0344643
_diffrn_orient_matrix_UB_31      -0.0328654
_diffrn_orient_matrix_UB_32      -0.0330287
_diffrn_orient_matrix_UB_33      -0.0192111
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_unetI/netI     0.1466
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 1
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12064
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 1
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_min         1.893
_exptl_absorpt_coefficient_mu    1.125
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.88704
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
        (compiled Aug  3 2011,13:03:54)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.1287
_exptl_crystal_size_mid          0.0933
_exptl_crystal_size_min          0.0537
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.69
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         5516
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0604P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1353
_reflns_number_gt                4050
_reflns_number_total             5516
_reflns_threshold_expression     'I > 2\s(I)'
_cod_duplicate_entry             7031813
_cod_data_source_file            c4dt01789g2.cif
_cod_data_source_block           n178
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C30 H33 Cl2 N1 O2 P2 Zn1'
_cod_database_code               7032457