Unexpected dimerisation of a 2H-azaphosphirene complex
Streubel, Rainer; Wilkens, Hendrik; Ruthe, Frank; Jones, Peter G.; Chemical Communications  (2000) 2453–; doi:10.1039/b007107m

data_7115144
_publ_section_title
;
 Unexpected dimerisation of a 2H-azaphosphirene complex
;
_journal_issue                   24
_journal_name_full               'Chemical Communications'
_journal_page_first              2453
_journal_paper_doi               10.1039/b007107m
_journal_year                    2000
_chemical_formula_sum            'C33 H48 N2 O5 P2 Si4 W'
_chemical_formula_weight         910.90
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.491(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.440(3)
_cell_length_b                   9.831(3)
_cell_length_c                   25.145(4)
_cell_measurement_reflns_used    47
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      2.5
_cell_volume                     4241.5(16)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       \w-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  0.1151
_diffrn_reflns_av_sigmaI/netI    0.2268
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            12772
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         3.03
_diffrn_standards_decay_%        2
_diffrn_standards_interval_count 247
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.949
_exptl_absorpt_correction_T_max  0.3231
_exptl_absorpt_correction_T_min  0.2557
_exptl_absorpt_correction_type   Psi-scans
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'cut prism'
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.162
_refine_diff_density_min         -0.712
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.763
_refine_ls_hydrogen_treatment    'all riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         7430
_refine_ls_number_restraints     171
_refine_ls_restrained_S_all      0.756
_refine_ls_R_factor_all          0.1494
_refine_ls_R_factor_gt           0.0537
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0581
_refine_ls_wR_factor_ref         0.0731
_reflns_number_gt                3410
_reflns_number_total             7430
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b007107m.txt
_cod_data_source_block           fidi1
_cod_original_cell_volume        4241.3(16)
_cod_original_sg_symbol_H-M      P2/n
_cod_original_formula_sum        'C33 H48 N2 O5 P2 Si4 W1'
_cod_database_code               7115144