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_4321712
_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_formula_moiety         'C28 H24 I P'
_chemical_formula_sum            'C28 H24 I P'
_chemical_formula_weight         518.34
_chemical_name_common            98277
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 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                 94.972(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.3318(1)
_cell_length_b                   10.1580(1)
_cell_length_c                   14.8414(3)
_cell_measurement_reflns_used    4341
_cell_measurement_temperature    193(2)
_cell_volume                     1101.18(3)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'SMART Platform CCD, Siemens'
_diffrn_measurement_method       omega-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0185
_diffrn_reflns_av_sigmaI/netI    0.0218
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5585
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    1.540
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.878426
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing (1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         1928
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0256
_refine_ls_R_factor_gt           0.0207
_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^)+(0.0321P)^2^+0.5099P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0539
_refine_ls_wR_factor_ref         0.0556
_reflns_number_gt                1705
_reflns_number_total             1928
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000838n_1.cif
_cod_data_source_block           98277
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multi-scans' was replaced
with the value 'multi-scan' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_database_code               4321712