Synthesis, Structures, and Multinuclear NMR Spectra of Tin(II) and Lead(II) Complexes of Tellurium-Containing Imidodiphosphinate Ligands: Preparation of Two Morphologies of Phase-Pure PbTe from a Single-Source Precursor
Jamie S. Ritch; Tristram Chivers; Kibriya Ahmad; Mohammad Afzaal; Paul O'Brien; Inorganic Chemistry 49 (2010) 1198–1205; doi:10.1021/ic9021728

data_4314724
_publ_contact_author_address
;
Department of Chemistry
University of Calgary
2500 University Drive NW
Calgary AB  T2N 1N4
Canada
;
_publ_contact_author_name        'Prof. Tristram Chivers'
_publ_section_title
;
 Synthesis, Structures, and Multinuclear NMR Spectra of Tin(II) and
 Lead(II) Complexes of Tellurium-Containing Imidodiphosphinate Ligands:
 Preparation of Two Morphologies of Phase-Pure PbTe from a Single-Source
 Precursor
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1198
_journal_page_last               1205
_journal_paper_doi               10.1021/ic9021728
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C24 H56 N2 P4 Pb Se2 Te2'
_chemical_formula_sum            'C24 H56 N2 P4 Pb Se2 Te2'
_chemical_formula_weight         1116.90
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 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                 120.15(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   34.625(7)
_cell_length_b                   9.7284(19)
_cell_length_c                   25.834(5)
_cell_measurement_reflns_used    35222
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.63
_cell_volume                     7525(3)
_computing_cell_refinement       'Nonius DENZO'
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'Nonius DENZO'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi\omega scans'
_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  0.0329
_diffrn_reflns_av_sigmaI/netI    0.0529
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            35222
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    8.126
_exptl_absorpt_correction_T_max  0.6001
_exptl_absorpt_correction_T_min  0.4422
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.972
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4224
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.515
_refine_diff_density_min         -4.222
_refine_diff_density_rms         0.309
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         6613
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0595
_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^)+(0.1046P)^2^+101.5145P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1606
_refine_ls_wR_factor_ref         0.1638
_reflns_number_gt                6243
_reflns_number_total             6613
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9021728_si_002_6.cif
_cod_data_source_block           Compound8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 
;
_cod_original_cell_volume        7524(3)
_cod_database_code               4314724