Synthesis of the first 1,2,3,4-azatriphospholene complex
Hoffmann, Nils; Wismach, Cathleen; Jones, Peter G.; Streubel, Rainer; Huy, Ngoc Hoa Tran; Mathey, François; Chemical Communications  (2002) 454–455; doi:10.1039/b110803b

data_7114362
_publ_section_title
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 Synthesis of the first 1,2,3,4-azatriphospholene complex
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_journal_issue                   5
_journal_name_full               'Chemical Communications'
_journal_page_first              454
_journal_page_last               455
_journal_paper_doi               10.1039/b110803b
_journal_year                    2002
_chemical_formula_sum            'C31 H21 N O5 P2 W'
_chemical_formula_weight         733.28
_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                 106.733(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6819(8)
_cell_length_b                   17.0312(10)
_cell_length_c                   13.7777(8)
_cell_measurement_reflns_used    45728
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     2849.8(3)
_computing_cell_refinement       'Bruker Saint'
_computing_data_collection       'Bruker Smart'
_computing_data_reduction        'Bruker Saint'
_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      133(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart 1000 CCD'
_diffrn_measurement_method       8.192
_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  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0188
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            44915
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         1.92
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.207
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.6029
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'cut tablet'
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.201
_refine_diff_density_min         -1.032
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    'P-H free, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         8327
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0217
_refine_ls_R_factor_gt           0.0181
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0319P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0483
_refine_ls_wR_factor_ref         0.0495
_reflns_number_gt                7452
_reflns_number_total             8327
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b110803b.txt
_cod_data_source_block           tuna
_cod_depositor_comments
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The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
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_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7114362