Pyrido-annellated diazaphospholenes and phospholenium ions
Benkő, Zoltán; Burck, Sebastian; Gudat, Dietrich; Nieger, Martin; Nyulászi, László; Shore, Nicholas; Dalton Transactions  (2008) 4937–4945; doi:10.1039/b804621b

data_7004242
_publ_section_title
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 Pyrido-annellated diazaphospholenes and phospholenium ions
;
_journal_issue                   36
_journal_name_full               'Dalton Transactions'
_journal_page_first              4937
_journal_page_last               4945
_journal_paper_doi               10.1039/b804621b
_journal_year                    2008
_chemical_formula_moiety         'C24 H40 N3 P Si2'
_chemical_formula_sum            'C24 H40 N3 P Si2'
_chemical_formula_weight         457.74
_chemical_name_common
;
3-(2,6-Diisopropylphenyl)-(1,5-a)pyridine-2-
hexamethyldisilazyl-(1,3,2)-diazaphospholene
;
_chemical_name_systematic
;
3-(2,6-Diisopropylphenyl)-[1,5-a]pyridine-2-hexamethyldisilazyl-
[1,3,2]-diazaphospholene
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                72.889(2)
_cell_angle_beta                 87.454(2)
_cell_angle_gamma                71.054(2)
_cell_formula_units_Z            2
_cell_length_a                   10.2893(3)
_cell_length_b                   10.4169(4)
_cell_length_c                   13.7477(6)
_cell_measurement_reflns_used    4774
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     1329.87(9)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       Collect
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    XP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'rotation in phi and omega, 2 deg.'
_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  0.0394
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14747
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    0.209
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       nlocks
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.303
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4681
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0437P)^2^+0.5602P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0940
_reflns_number_gt                3829
_reflns_number_total             4681
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b804621b.txt
_cod_data_source_block           dg022_hy_compound_3a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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_database_code               7004242