Synthesis and X-ray Structures of Dilithium Complexes of the Phosphonate Anions [PhP(E)(NtBu)2]2- (E = O, S, Se, Te) and Dimethylaluminum Derivatives of [PhP(E)(NtBu)(NHtBu)]- (E = S, Se)
Glen G. Briand; Tristram Chivers; Mark Krahn; Masood Parvez; Inorganic Chemistry 41 (2002) 6808–6815; doi:10.1021/ic020471h

data_4319014
_publ_contact_author_email       ' parvez@ucalgary.ca '
_publ_contact_author_fax         ' (403)289-9488 '
_publ_contact_author_phone       ' (403)220-5348 '
_publ_section_title
;
 Synthesis and X-ray Structures of Dilithium Complexes of the Phosphonate
 Anions [PhP(E)(NtBu)2]2- (E = O, S, Se, Te) and Dimethylaluminum
 Derivatives of [PhP(E)(NtBu)(NHtBu)]- (E = S, Se)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6808
_journal_page_last               6815
_journal_paper_doi               10.1021/ic020471h
_journal_volume                  41
_journal_year                    2002
_chemical_compound_source        'synthesized by authors '
_chemical_formula_sum            'C22 H39 Li2 N2 O2 P Se'
_chemical_formula_weight         487.36
_chemical_melting_point          ' ? '
_chemical_name_common            ' ? '
_chemical_name_systematic        ' ? '
_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
_cell_angle_alpha                89.0090(10)
_cell_angle_beta                 73.1940(10)
_cell_angle_gamma                66.3900(10)
_cell_formula_units_Z            2
_cell_length_a                   9.41300(10)
_cell_length_b                   10.2438(2)
_cell_length_c                   15.1293(2)
_cell_measurement_reflns_used    10652
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.0
_cell_volume                     1271.54(4)
_computing_cell_refinement       'HKL DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction        'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'TEXSAN (M. S. C., 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SAPI91 (Fan, 1991)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Nonius KappaCCD Diffractometer'
_diffrn_measurement_method       ' \w & \f '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0115
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10652
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         4.21
_diffrn_standards_decay_%        ' < 0.1 '
_exptl_absorpt_coefficient_mu    1.558
_exptl_absorpt_correction_T_max  0.6967
_exptl_absorpt_correction_T_min  0.6522
_exptl_absorpt_correction_type   'Multi-scan method'
_exptl_absorpt_process_details   '(SORTAV: Blessing, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.051
_refine_diff_density_min         -1.011
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         5732
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.048P)^2^+1.453P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.0978
_reflns_number_gt                5455
_reflns_number_total             5732
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020471h_5.cif
_cod_data_source_block           Compound_2c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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        1271.54(3)
_cod_original_sg_symbol_H-M      ' P -1 '
_cod_database_code               4319014