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_7114361
_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            'C52 H42 N O11 P4 W2'
_chemical_formula_weight         1348.45
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                85.462(3)
_cell_angle_beta                 79.491(3)
_cell_angle_gamma                63.886(3)
_cell_formula_units_Z            2
_cell_length_a                   13.5051(8)
_cell_length_b                   14.5592(11)
_cell_length_c                   14.8611(11)
_cell_measurement_reflns_used    7007
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2.75
_cell_volume                     2579.7(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_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker AXS Smart 1000CCD'
_diffrn_measurement_method       '\w- & \f-scan'
_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  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            54053
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    4.639
_exptl_absorpt_correction_T_max  0.7733
_exptl_absorpt_correction_T_min  0.4884
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.736
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1314
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.458
_refine_diff_density_min         -1.097
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         15022
_refine_ls_number_restraints     125
_refine_ls_restrained_S_all      0.943
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0290P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0557
_refine_ls_wR_factor_ref         0.0594
_reflns_number_gt                11600
_reflns_number_total             15022
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b110803b.txt
_cod_data_source_block           nils
_cod_depositor_comments
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The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'heavy-atom' was changed to
'heavy'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
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_cod_database_code               7114361