Neutral Molecular Pd6Hexagons Using κ3-P2O-Terdentate Ligands
Elsegood, Mark R. J.; Smith, Martin B.; Staniland, Paul M.; Inorganic Chemistry 45 (2006) 6761–6770; doi:10.1021/ic060629o

data_4332657
_publ_section_title
;
 Neutral Molecular Pd6Hexagons Using \k3-P2O-Terdentate Ligands
;
_journal_issue                   17
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6761
_journal_page_last               6770
_journal_paper_doi               10.1021/ic060629o
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C221 H180 Cl51 D17 I6 N6 O18 P12 Pd6'
_chemical_formula_weight         6821.34
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :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            9
_cell_length_a                   50.7094(13)
_cell_length_b                   50.7094(13)
_cell_length_c                   27.6292(10)
_cell_measurement_reflns_used    36860
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.48
_cell_measurement_theta_min      2.15
_cell_volume                     61528(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_sigmaI/netI    0.0557
_diffrn_reflns_limit_h_max       68
_diffrn_reflns_limit_h_min       -67
_diffrn_reflns_limit_k_max       66
_diffrn_reflns_limit_k_min       -68
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            182777
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.15
_diffrn_reflns_theta_min         0.80
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.688
_exptl_absorpt_correction_T_max  0.877
_exptl_absorpt_correction_T_min  0.762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.01, Sheldrick, G.M., (2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             30150
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_platon_squeeze_details
; ?
R=6.7% before squueze. 6 extra CDCl~3~ per hexamer added to the
formula.
;
_refine_diff_density_max         1.392
_refine_diff_density_min         -1.313
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1382
_refine_ls_number_reflns         33687
_refine_ls_number_restraints     271
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0957P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1557
_refine_ls_wR_factor_ref         0.1722
_reflns_number_gt                21112
_reflns_number_total             33687
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic060629osup1.cif
_cod_data_source_block           9
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               4332657