Synthesis and Characterization of Pd(0) and Pt(0) Metallocryptands Encapsulating Tl+ Ion
Vincent J. Catalano; Byron L. Bennett; Renante L. Yson; Bruce C. Noll; Journal of the American Chemical Society 122 (2000) 10056–10062; doi:10.1021/ja001672s

data_4116188
_publ_contact_author_address
;
Department of Chemistry
University of Nevada
Reno, NV  89557
;
_publ_contact_author_email       vjc@unr.edu
_publ_contact_author_name        'Professor Vincent J. Catalano'
_publ_contact_author_phone       '775 784 1329'
_publ_section_title
;
 Synthesis and Characterization of Pd(0) and Pt(0) Metallocryptands
 Encapsulating Tl+ Ion
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10056
_journal_page_last               10062
_journal_paper_doi               10.1021/ja001672s
_journal_volume                  122
_journal_year                    2000
_chemical_formula_sum            'C126 H78 Cl0 N7 O7 P6 Pd2 Tl'
_chemical_formula_weight         2404.94
_chemical_name_common            4
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           167
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   19.3462(2)
_cell_length_b                   19.3462(2)
_cell_length_c                   51.7863(8)
_cell_measurement_reflns_used    7529
_cell_measurement_temperature    138(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      1.45
_cell_volume                     16785.6(4)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      138(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.069
_diffrn_reflns_av_sigmaI/netI    0.039
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       72
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            49051
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    1.890
_exptl_absorpt_correction_T_max  0.81
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_description       Block
_exptl_crystal_F_000             7212
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.949
_refine_diff_density_min         -1.647
_refine_diff_density_rms         0.309
_refine_ls_extinction_coef       0.00046(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.579
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         5473
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.603
_refine_ls_R_factor_all          0.1167
_refine_ls_R_factor_gt           0.0816
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2356
_refine_ls_wR_factor_ref         0.2498
_reflns_number_gt                3703
_reflns_number_total             5473
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja001672s_1.cif
_cod_data_source_block           bc322
_cod_original_cell_volume        16786.2(2)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4116188