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_4319011
_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            'C77 H136 Li10 N8 O9 P4'
_chemical_formula_weight         1511.22
_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                102.230(1)
_cell_angle_beta                 111.629(1)
_cell_angle_gamma                99.731(1)
_cell_formula_units_Z            2
_cell_length_a                   15.8348(2)
_cell_length_b                   15.9927(2)
_cell_length_c                   20.2186(3)
_cell_measurement_reflns_used    47285
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      1.0
_cell_volume                     4476.28(12)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0510
_diffrn_reflns_av_sigmaI/netI    0.0903
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            47285
_diffrn_reflns_theta_full        30.04
_diffrn_reflns_theta_max         30.04
_diffrn_reflns_theta_min         1.35
_diffrn_standards_decay_%        ' < 0.1 '
_exptl_absorpt_coefficient_mu    0.138
_exptl_absorpt_correction_T_max  0.9864
_exptl_absorpt_correction_T_min  0.9598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SORTAV: Blessing, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.627
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     972
_refine_ls_number_reflns         25974
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1304
_refine_ls_R_factor_gt           0.0655
_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^)+(0.09P)^2^+1.02P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1647
_refine_ls_wR_factor_ref         0.1962
_reflns_number_gt                14857
_reflns_number_total             25974
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020471h_2.cif
_cod_data_source_block           Compound_2a.Li2O
_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        4476.27(10)
_cod_original_sg_symbol_H-M      ' P -1 '
_cod_database_code               4319011