Ambident σ- and π-donor ability of a neutral 10π-aromatic phosphoniobenzophospholide
Gudat, Dietrich; Häp, Stefan; Szarvas, Laszlo; Nieger, Martin; Chemical Communications  (2000) 1637–; doi:10.1039/b005130f

data_7111042
_publ_section_title
;
 Ambident \s- and \p-donor ability of a neutral 10\p-aromatic
 phosphoniobenzophospholide
;
_journal_issue                   17
_journal_name_full               'Chemical Communications'
_journal_page_first              1637
_journal_paper_doi               10.1039/b005130f
_journal_year                    2000
_chemical_formula_sum            'C31 H20 Cr O5 P2'
_chemical_formula_weight         586.41
_chemical_name_systematic
; 
 Pentacarbonyl-(1-triphenylphosphonio-benzo-[c]-phospholide)chromium(0) 
;
_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                111.151(2)
_cell_angle_beta                 93.476(2)
_cell_angle_gamma                110.126(2)
_cell_formula_units_Z            2
_cell_length_a                   10.2695(4)
_cell_length_b                   11.0128(4)
_cell_length_c                   13.7391(4)
_cell_measurement_reflns_used    18369
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.5
_cell_measurement_theta_min      2.5
_cell_volume                     1330.03(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      123(2)
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_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  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0571
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18922
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    0.591
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         6253
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0349P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0839
_reflns_number_gt                4815
_reflns_number_total             6253
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b005130fsup1.cif
_cod_data_source_block           compound_3
_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 
;
_cod_original_cell_volume        1330.03(8)
_cod_original_sg_symbol_H-M      'P-1 (no.2)'
_cod_database_code               7111042