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_4335946
_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         'C144 H96 N24 O12 Pd12, 3(C H2 Cl2)'
_chemical_formula_sum            'C147 H102 Cl6 N24 O12 Pd12'
_chemical_formula_weight         3886.10
_chemical_melting_point          350
_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   difmap
_atom_sites_solution_primary     other
_atom_sites_solution_secondary   difmap
_audit_creation_date             13-03-05
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   18.1579(4)
_cell_length_b                   18.1579(4)
_cell_length_c                   76.3832(17)
_cell_measurement_reflns_used    7782
_cell_measurement_temperature    150
_cell_measurement_theta_max      63
_cell_measurement_theta_min      3
_cell_volume                     21810.2(8)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.062
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       87
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7782
_diffrn_reflns_theta_full        62.820
_diffrn_reflns_theta_max         62.820
_diffrn_reflns_theta_min         2.869
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.230
_exptl_absorpt_correction_T_max  0.46
_exptl_absorpt_correction_T_min  0.26
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.775
_exptl_crystal_description       block
_exptl_crystal_F_000             11412
_exptl_crystal_size_max          0.118
_exptl_crystal_size_mid          0.114
_exptl_crystal_size_min          0.059
_platon_squeeze_details
;
;
_refine_diff_density_max         1.42
_refine_diff_density_min         -1.45
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         7734
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.0024036
_refine_ls_shift/su_mean         0.0000324
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.101E+04 0.146E+04 775. 246. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0842
_refine_ls_wR_factor_gt          0.0749
_refine_ls_wR_factor_ref         0.0842
_reflns_limit_h_max              10
_reflns_limit_h_min              -20
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              87
_reflns_limit_l_min              0
_reflns_number_gt                6315
_reflns_number_total             7782
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.52
_oxford_diffrn_Wilson_scale      5.93
_oxford_refine_ls_r_factor_ref   0.0513
_oxford_refine_ls_scale          0.4296(3)
_oxford_reflns_number_all        7734
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'CM29_AcDcm_MeOH in R-3'
_cod_data_source_file            ic401253q_si_002.cif
_cod_data_source_block           1
_cod_original_cell_volume        21810.1(8)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4335946
_iucr_refine_instruction_details_constraints
;
BLOC SCALE X'S U'S 
RIDE C   (  17,X'S) H   ( 171,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   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  27,X'S) H   ( 271,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) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) 
RIDE C   (  57,X'S) H   ( 571,X'S) 
RIDE C   (  58,X'S) H   ( 581,X'S) 
RIDE C   (  61,X'S) H   ( 611,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) 
RIDE C   (  64,X'S) H   ( 641,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) H   ( 662,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
END                                                                             
;