Chalcogeno-urea Ligands on a Phosphadiazonium Lewis Acceptor: A New Synthetic Approach to Ch-P Bonds (Ch = O, S, Se)
Neil Burford; Andrew D. Phillips; Heather A. Spinney; Katherine N. Robertson; T. Stanley Cameron; Robert McDonald; Inorganic Chemistry 42 (2003) 4949–4954; doi:10.1021/ic034182k

data_4313946
_publ_contact_author_address
;
Department of Chemistry
Dalhousie University
Halifax, Nova Scotia
B3H 4J3
;
_publ_contact_author_email       ' Neil.Burford@dal.ca '
_publ_contact_author_fax         ' 902-494-1310 '
_publ_contact_author_name        'Neil Burford'
_publ_contact_author_phone       ' 902-494-3190 '
_publ_section_title
;
 Chalcogeno-urea Ligands on a Phosphadiazonium Lewis Acceptor: A New
 Synthetic Approach to Ch-P Bonds (Ch = O, S, Se)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4949
_journal_page_last               4954
_journal_paper_doi               10.1021/ic034182k
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C34 H45 F3 N3 O4 P S'
_chemical_formula_weight         679.76
_chemical_name_systematic
;
 ?
;
_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      2.2
_audit_creation_date             2002-09-19T23:17:40-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 103.611(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.569(2)
_cell_length_b                   11.2697(10)
_cell_length_c                   13.5349(12)
_cell_measurement_temperature    193(2)
_cell_volume                     3642.4(5)
_computing_cell_refinement       'Bruker SMART (Bruker, 1997)'
_computing_data_collection       'Bruker SMART (Bruker, 1997)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomere et al., 1994)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
;
Bruker P4/RA diffractometer/SMART 1000 CCD area detector
;
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18056
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         1.71
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.187
_exptl_absorpt_correction_T_max  0.9565
_exptl_absorpt_correction_T_min  0.9139
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.24
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.53
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.02
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         6398
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.02
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.0802P)^2^+2.1649P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1342
_refine_ls_wR_factor_ref         0.1445
_reflns_number_gt                5222
_reflns_number_total             6398
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034182ksi20030218_083705_1.cif
_cod_data_source_block           '[Mes*NP.OU]OTf'
_cod_original_cell_volume        3642.4(6)
_cod_original_sg_symbol_H-M      'P 1 21/n 1'
_cod_database_code               4313946