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_4335947
_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         'C122 H82 N22 O12 Pd10, 5(C6 H6)'
_chemical_formula_sum            'C152 H112 N22 O12 Pd10'
_chemical_formula_weight         3502.70
_chemical_melting_point          450
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             13-03-15
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 113.678(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.620(6)
_cell_length_b                   37.337(9)
_cell_length_c                   16.594(4)
_cell_measurement_reflns_used    14313
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      4
_cell_volume                     15105(6)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_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    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  Unknown
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.060
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14313
_diffrn_reflns_theta_full        28.196
_diffrn_reflns_theta_max         28.196
_diffrn_reflns_theta_min         3.000
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.225
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.59
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_description       plate
_exptl_crystal_F_000             6936
_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.202
_exptl_crystal_size_min          0.033
_platon_squeeze_details
;
;
_refine_diff_density_max         2.87
_refine_diff_density_min         -2.03
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9426
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     917
_refine_ls_number_reflns         14252
_refine_ls_number_restraints     1477
_refine_ls_R_factor_all          0.1100
_refine_ls_R_factor_gt           0.0643
_refine_ls_shift/su_max          0.0311095
_refine_ls_shift/su_mean         0.0025084
_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: 
 4.41 5.22 1.38 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1693
_refine_ls_wR_factor_gt          0.1318
_refine_ls_wR_factor_ref         0.1687
_reflns_limit_h_max              29
_reflns_limit_h_min              -32
_reflns_limit_k_max              45
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                9123
_reflns_number_total             14313
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.1096
_oxford_refine_ls_scale          0.029204(2)
_oxford_reflns_number_all        14270
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title '2cy1 in C2/c'
_cod_data_source_file            ic401253q_si_003.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4335947
_iucr_refine_instruction_details_constraints
;
FULL PD(1,X'S,U'S) UNTIL C(83) 
CONT C(84,X'S,U[ISO]) UNTIL C(98) 
CONT N(481,X'S,U'S) UNTIL C(591) 
EQUIVALENCE PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
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) 
RIDE C   (  23,X'S) H   ( 231,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 N   (  32,X'S) H   ( 321,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   (  40,X'S) H   ( 401,X'S) 
RIDE C   (  44,X'S) H   ( 441,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   (  64,X'S) H   ( 641,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) 
RIDE C   (  67,X'S) H   ( 671,X'S) 
RIDE C   (  68,X'S) H   ( 681,X'S) 
RIDE C   (  69,X'S) H   ( 691,X'S) 
RIDE C   (  70,X'S) H   ( 701,X'S) 
RIDE C   (  71,X'S) H   ( 711,X'S) 
RIDE C   (  76,X'S) H   ( 761,X'S) 
RIDE C   (  77,X'S) H   ( 771,X'S) 
RIDE C   (  78,X'S) H   ( 781,X'S) 
RIDE C   (  79,X'S) H   ( 791,X'S) 
RIDE C   (  80,X'S) H   ( 801,X'S) 
RIDE C   (  81,X'S) H   ( 811,X'S) 
RIDE C   (  82,X'S) H   ( 821,X'S) 
RIDE C   (  83,X'S) H   ( 831,X'S) 
RIDE C   (  84,X'S) H   ( 841,X'S) 
RIDE C   (  85,X'S) H   ( 851,X'S) 
RIDE C   (  86,X'S) H   ( 861,X'S) 
RIDE C   (  87,X'S) H   ( 871,X'S) 
RIDE C   (  88,X'S) H   ( 881,X'S) 
RIDE C   (  89,X'S) H   ( 891,X'S) 
RIDE C   (  90,X'S) H   ( 901,X'S) 
RIDE C   (  91,X'S) H   ( 911,X'S) 
RIDE C   (  92,X'S) H   ( 921,X'S) 
RIDE C   (  93,X'S) H   ( 931,X'S) 
RIDE C   (  94,X'S) H   ( 941,X'S) 
RIDE C   (  95,X'S) H   ( 951,X'S) 
RIDE C   (  96,X'S) H   ( 961,X'S) 
RIDE C   (  97,X'S) H   ( 971,X'S) 
RIDE C   (  98,X'S) H   ( 981,X'S) 
RIDE C   ( 521,X'S) H   (5211,X'S) 
RIDE C   ( 511,X'S) H   (5111,X'S) 
RIDE C   ( 501,X'S) H   (5011,X'S) 
RIDE C   ( 491,X'S) H   (4911,X'S) 
RIDE C   ( 490,X'S) H   (4901,X'S) 
RIDE C   ( 500,X'S) H   (5001,X'S) 
RIDE C   ( 510,X'S) H   (5101,X'S) 
RIDE C   ( 520,X'S) H   (5201,X'S) 
RIDE C   ( 590,X'S) H   (5901,X'S) 
RIDE C   ( 580,X'S) H   (5801,X'S) 
RIDE C   ( 570,X'S) H   (5701,X'S) 
RIDE C   ( 560,X'S) H   (5601,X'S) 
RIDE C   ( 561,X'S) H   (5611,X'S) 
RIDE C   ( 571,X'S) H   (5711,X'S) 
RIDE C   ( 581,X'S) H   (5811,X'S) 
RIDE C   ( 591,X'S) H   (5911,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
DIST 0.0, .001 = MEAN N(480) TO C(490), N(480) TO C(530) 
DIST 0.0, .001 = MEAN C(490) TO C(500), C(530) TO C(520) 
DIST 0.0, .001 = MEAN C(500) TO C(510), C(520) TO C(510) 
ANGLE 0.0, .02 = MEAN N(480) TO C(490) TO C(500), 
CONTINUE           N(480) TO C(530) TO C(520) 
ANGLE 0.0, .02 = MEAN C(490) TO C(500) TO C(510), 
CONTINUE           C(530) TO C(520) TO C(510) 
DIST 0.0, .001 = MEAN N(481) TO C(531), N(481) TO C(491) 
DIST 0.0, .001 = MEAN C(531) TO C(521), C(491) TO C(501) 
DIST 0.0, .001 = MEAN C(521) TO C(511), C(501) TO C(511) 
ANGLE 0.0, .02 = MEAN N(481) TO C(531) TO C(521), 
CONTINUE           N(481) TO C(491) TO C(501) 
ANGLE 0.0, .02 = MEAN C(531) TO C(521) TO C(511), 
CONTINUE           C(491) TO C(501) TO C(511) 
DIST 0.0, .001 = MEAN C(541) TO C(551), C(541) TO C(591) 
DIST 0.0, .001 = MEAN C(551) TO C(561), C(591) TO C(581) 
DIST 0.0, .001 = MEAN C(561) TO C(571), C(581) TO C(571) 
ANGLE 0.0, .02 = MEAN C(541) TO C(551) TO C(561), 
CONTINUE           C(541) TO C(591) TO C(581) 
ANGLE 0.0, .02 = MEAN C(551) TO C(561) TO C(571), 
CONTINUE           C(591) TO C(581) TO C(571) 
DIST 0.0, .001 = MEAN C(540) TO C(590), C(540) TO C(550) 
DIST 0.0, .001 = MEAN C(590) TO C(580), C(550) TO C(560) 
DIST 0.0, .001 = MEAN C(580) TO C(570), C(560) TO C(570) 
ANGLE 0.0, .02 = MEAN C(540) TO C(590) TO C(580), 
CONTINUE           C(540) TO C(550) TO C(560) 
ANGLE 0.0, .02 = MEAN C(590) TO C(580) TO C(570), 
CONTINUE           C(550) TO C(560) TO C(570) 
DIST 0.0, .001 = MEAN C(87) TO C(88), C(87) TO C(92) 
DIST 0.0, .001 = MEAN C(88) TO C(89), C(92) TO C(91) 
DIST 0.0, .001 = MEAN C(89) TO C(90), C(91) TO C(90) 
ANGLE 0.0, .02 = MEAN C(87) TO C(88) TO C(89), 
CONTINUE           C(87) TO C(92) TO C(91) 
ANGLE 0.0, .02 = MEAN C(88) TO C(89) TO C(90), 
CONTINUE           C(92) TO C(91) TO C(90) 
DIST 0.0, .001 = MEAN C(93) TO C(94), C(93) TO C(98) 
DIST 0.0, .001 = MEAN C(94) TO C(95), C(98) TO C(97) 
DIST 0.0, .001 = MEAN C(95) TO C(96), C(97) TO C(96) 
ANGLE 0.0, .02 = MEAN C(93) TO C(94) TO C(95), 
CONTINUE           C(93) TO C(98) TO C(97) 
ANGLE 0.0, .02 = MEAN C(94) TO C(95) TO C(96), 
CONTINUE           C(98) TO C(97) TO C(96) 
DIST 1.39, 0.01 = C(84) TO C(85), C(85) TO C(86) 
SIMU 0.01 PART(1001) PART(1002) 
DELU 0.01 PART(1001) PART(1002) 
REM   SHIFTLIMIT   START (DO NOT REMOVE THIS LINE) 
LIMIT      0.01000000 U[ISO] 
LIMIT      0.01000000 X 
LIMIT      0.01000000 y
LIMIT      0.01000000 Z 
LIMIT      0.01000000 U[11] 
LIMIT      0.01000000 U[22] 
LIMIT      0.01000000 U[33] 
LIMIT      0.01000000 U[12] 
LIMIT      0.01000000 U[13] 
LIMIT      0.01000000 U[23] 
REM   SHIFTLIMIT   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;