1,2-Azaphosphol-5-ene Complexes through Metal-Assisted Synthesis
Streubel, Rainer; Wilkens, Hendrik; Ruthe, Frank; Jones, Peter G.; Organometallics 25 (2006) 4830–; doi:10.1021/om060344j

data_4075527
_publ_section_title
;
 1,2-Azaphosphol-5-ene Complexes through Metal-Assisted Synthesis
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              4830
_journal_paper_doi               10.1021/om060344j
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C23 H37 N2 O7 P Si2 W'
_chemical_formula_weight         724.55
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.50(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.049(3)
_cell_length_b                   17.105(4)
_cell_length_c                   17.623(10)
_cell_measurement_reflns_used    54
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      11.5
_cell_measurement_theta_min      10
_cell_volume                     3015(2)
_computing_cell_refinement       'Stoe DIF4'
_computing_data_collection       'Stoe DIF4'
_computing_data_reduction        'Stoe REDU4'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Stoe STADI-4'
_diffrn_measurement_method       \w/\q-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0393
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7116
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.13
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.004
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.489
_exptl_absorpt_correction_type   Psi-scans
_exptl_absorpt_process_details   XEMP
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.089
_refine_diff_density_min         -1.803
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    'rigid methyls, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         5306
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0407P)^2^+4.0731P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0822
_reflns_number_gt                4529
_reflns_number_total             5306
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060344jsi20060425_125952.cif
_cod_data_source_block           najah
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4075527