Tripodal 4-Pyridyl-Derived Host Ligands and Their Metallo-Supramolecular Chemistry: Stella Octangula and Bowl-Shaped Assemblies
Tanya K. Ronson; Christopher Carruthers; Julie Fisher; Thierry Brotin; Lindsay P. Harding; Pierre J. Rizkallah; Michaele J. Hardie; Inorganic Chemistry 49 (2010) 675–685; doi:10.1021/ic901972h

data_4314574
_publ_section_title
;
 Tripodal 4-Pyridyl-Derived Host Ligands and Their Metallo-Supramolecular
 Chemistry: Stella Octangula and Bowl-Shaped Assemblies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              675
_journal_page_last               685
_journal_paper_doi               10.1021/ic901972h
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C184 H209 N15 O43.5 Pd8 S3'
_chemical_formula_weight         4274.04
_chemical_name_systematic
; 
 tetrakis(Tris(4-pyridylmethyl)cyclotriguaiacylene)trispalladium nitrate
;
_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                 100.545(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   43.49(3)
_cell_length_b                   28.10(3)
_cell_length_c                   40.83(4)
_cell_measurement_temperature    150(2)
_cell_volume                     49054(8)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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      150(2)
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Bruker D8 diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS, Station 16.2SMX'
_diffrn_radiation_type           'synchrotron, l = 0.7977'
_diffrn_reflns_av_R_equivalents  0.1208
_diffrn_reflns_av_sigmaI/netI    0.1250
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            70813
_diffrn_reflns_theta_full        17.75
_diffrn_reflns_theta_max         17.75
_diffrn_reflns_theta_min         3.19
_exptl_absorpt_coefficient_mu    0.659
_exptl_absorpt_correction_T_max  0.9615
_exptl_absorpt_correction_T_min  0.9076
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             17456
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.513
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1123
_refine_ls_number_reflns         15312
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1491
_refine_ls_R_factor_gt           0.1122
_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^)+(0.1966P)^2^+188.8243P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3009
_refine_ls_wR_factor_ref         0.3267
_reflns_number_gt                9929
_reflns_number_total             15312
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901972h_si_001_5.cif
_cod_data_source_block           Pd3(L3)4
_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 

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        49058(79)
_cod_original_formula_sum        'C184 H209 N15 O43.50 Pd8 S3'
_cod_database_code               4314574