Pairwise Assembly of Organopalladium(II) Units with Cyanurato(3-) and Trithiocyanurato(3-) Ligands: Formation of Chiral Pd12, Pd10, and Pd9 Cage-Molecules
Claire A. Murray; Christine J. Cardin; Barnaby W. Greenland; Andrew Swift; Howard M. Colquhoun; Inorganic Chemistry 52 (2013) 10424–10430; doi:10.1021/ic401253q

data_4335948
_publ_contact_author_address
; 
Department of Chemistry
University of Reading
Whiteknights
Reading
RG6 6AD 
;
_publ_contact_author_email       h.m.colquhoun@reading.ac.uk
_publ_contact_author_fax         '+44 1183 786717'
_publ_contact_author_name        'Howard M. Colquhoun'
_publ_contact_author_phone       '+44 1183 786717'
_publ_section_title
;
 Pairwise Assembly of Organopalladium(II) Units with Cyanurato(3-) and
 Trithiocyanurato(3-) Ligands: Formation of Chiral Pd12, Pd10, and Pd9
 Cage-Molecules
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10424
_journal_page_last               10430
_journal_paper_doi               10.1021/ic401253q
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         '2(C120 H144 N24 O12 Pd12), C H Cl3'
_chemical_formula_sum            'C241 H289 Cl3 N48 O24 Pd24'
_chemical_formula_weight         6902.61
_space_group_IT_number           205
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P a -3'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             13-03-02
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.4972(2)
_cell_length_b                   29.4972(2)
_cell_length_c                   29.4972(2)
_cell_measurement_reflns_used    14765
_cell_measurement_temperature    150
_cell_measurement_theta_max      32
_cell_measurement_theta_min      2
_cell_volume                     25665.1(3)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'Gemini, (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.106
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            175578
_diffrn_reflns_theta_full        30.114
_diffrn_reflns_theta_max         32.380
_diffrn_reflns_theta_min         2.392
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.735
_exptl_absorpt_correction_T_max  0.70
_exptl_absorpt_correction_T_min  0.60
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.786
_exptl_crystal_description       block
_exptl_crystal_F_000             13672
_exptl_crystal_size_max          0.303
_exptl_crystal_size_mid          0.287
_exptl_crystal_size_min          0.209
_refine_diff_density_max         3.09
_refine_diff_density_min         -2.14
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.3384
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     519
_refine_ls_number_reflns         14736
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.1170
_refine_ls_R_factor_gt           0.0842
_refine_ls_shift/su_max          0.0016727
_refine_ls_shift/su_mean         0.0000359
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.10P)^2^ + 0.00P] 
 ,where P=p(6)*max(Fo^2^,0) + (1-p(6))Fc^2^ 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2173
_refine_ls_wR_factor_gt          0.2017
_refine_ls_wR_factor_ref         0.2173
_reflns_limit_h_max              0
_reflns_limit_h_min              -31
_reflns_limit_k_max              30
_reflns_limit_k_min              0
_reflns_limit_l_max              44
_reflns_limit_l_min              2
_reflns_number_gt                11138
_reflns_number_total             14765
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.62
_oxford_diffrn_Wilson_scale      24.70
_oxford_refine_ls_r_factor_ref   0.1170
_oxford_refine_ls_scale          0.21617(19)
_oxford_reflns_number_all        14736
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title CM5
_cod_data_source_file            ic401253q_si_004.cif
_cod_data_source_block           1
_cod_original_cell_volume        25665.0(3)
_cod_original_sg_symbol_H-M      'P a -3 '
_cod_database_code               4335948
_iucr_refine_instruction_details_constraints
;
BLOC SCALE X'S U'S 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) H   ( 223,X'S) H   ( 222,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) H   ( 233,X'S) H   ( 232,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) H   ( 282,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 353,X'S) H   ( 352,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 363,X'S) H   ( 362,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) H   ( 382,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) H   ( 453,X'S) H   ( 452,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) H   ( 463,X'S) H   ( 462,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) H   ( 483,X'S) H   ( 482,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) H   ( 492,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) H   ( 563,X'S) H   ( 562,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
END                                                                             
;