The First Noncoordinated Phosphonium Diylide, [Me2P(C13H8)2]-, and Its Ylidic and Cationic Counterparts: Synthesis, Structural Characterization, and Interaction with the Heavy Group 2 Metals
Erik D. Brady; Timothy P. Hanusa; Maren Pink; Victor G. Young; Inorganic Chemistry 39 (2000) 6028–6037; doi:10.1021/ic000838n

data_4321713
_publ_section_title
;
 The First Noncoordinated Phosphonium Diylide, [Me2P(C13H8)2]-, and Its
 Ylidic and Cationic Counterparts: Synthesis, Structural Characterization,
 and Interaction with the Heavy Group 2 Metals
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6028
_journal_page_last               6037
_journal_paper_doi               10.1021/ic000838n
_journal_volume                  39
_journal_year                    2000
_chemical_compound_source        'Prof. T. Hanusa - Vanderbilt University'
_chemical_formula_sum            'C52 H70 Ca I O6 P'
_chemical_formula_weight         989.03
_chemical_name_common            99331a
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 110.658(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.0619(7)
_cell_length_b                   22.6419(13)
_cell_length_c                   17.9082(10)
_cell_measurement_temperature    173(2)
_cell_volume                     4955.7(5)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_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  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0390
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            38232
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    0.829
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.737
_exptl_absorpt_correction_type   mutli-scans
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_description       Block
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.782
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.040
_refine_ls_goodness_of_fit_obs   1.165
_refine_ls_matrix_type           full
_refine_ls_number_parameters     596
_refine_ls_number_reflns         11257
_refine_ls_number_restraints     548
_refine_ls_restrained_S_all      1.051
_refine_ls_restrained_S_obs      1.172
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_obs          0.0408
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0604P)^2^+0.2664P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1152
_refine_ls_wR_factor_obs         0.1033
_reflns_number_observed          7403
_reflns_number_total             11257
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000838n_2.cif
_cod_data_source_block           99331a
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0604P)^2^+0.2664P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0604P)^2^+0.2664P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4321713