Supramolecular Macrocyclic Pd(II) and Pt(II) Squares and Rectangles with Aryldithiolate Ligands and their Excellent Catalytic Activity in Suzuki C-C Coupling Reaction.
Vivekananda, K. V.; Dey, S.; Maity, D. K.; Bhuvanesh, N.; Jain, V. K.; Inorganic chemistry 54 (2015) 10153–10162; doi:10.1021/acs.inorgchem.5b00806

data_4344226
_publ_section_title
;
 Supramolecular Macrocyclic Pd(II) and Pt(II) Squares and Rectangles with
 Aryldithiolate Ligands and their Excellent Catalytic Activity in Suzuki
 C-C Coupling Reaction.
;
_journal_issue                   21
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10153
_journal_page_last               10162
_journal_paper_doi               10.1021/acs.inorgchem.5b00806
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety
'C240 H224 P16 Pd8 S8, 4(C F3 O3 S), 2(C3 H6 O)'
_chemical_formula_sum            'C250 H236 F12 O14 P16 Pd8 S12'
_chemical_formula_weight         5423.81
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-06-20
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                61.8080(10)
_cell_angle_beta                 71.3300(10)
_cell_angle_gamma                68.6400(10)
_cell_formula_units_Z            1
_cell_length_a                   17.2155(16)
_cell_length_b                   21.975(2)
_cell_length_c                   22.457(2)
_cell_measurement_reflns_used    9223
_cell_measurement_temperature    110.15
_cell_measurement_theta_max      27.453
_cell_measurement_theta_min      2.175
_cell_volume                     6859.2(11)
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      110.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            127933
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.539
_diffrn_reflns_theta_min         1.046
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.757
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0662 before and 0.0566 after correction.
The Ratio of minimum to maximum transmission is 0.8894.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_description       block
_exptl_crystal_F_000             2756
_exptl_crystal_size_max          0.484
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.082
_refine_diff_density_max         2.138
_refine_diff_density_min         -1.690
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1407
_refine_ls_number_reflns         31331
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0533
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0233P)^2^+31.5397P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1256
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24781
_reflns_number_total             31331
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00806_si_002.cif
_cod_data_source_block           sd38_sq
_cod_depositor_comments
'Adding full bibliography for 4344224--4344226.cif.'
_cod_original_cell_volume        6859.3(11)
_cod_database_code               4344226
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.941
_shelx_estimated_absorpt_t_min   0.711
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C27(H27A,H27B), C34(H34A,H34B), C35(H35A,H35B),
 C36(H36A,H36B), C61(H61A,H61B), C62(H62A,H62B), C87(H87A,H87B), C94(H94A,H94B),
  C95(H95A,H95B), C96(H96A,H96B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22),
  C23(H23), C24(H24), C25(H25), C26(H26), C29(H29), C30(H30), C32(H32),
 C33(H33), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C44(H44), C45(H45),
  C46(H46), C47(H47), C48(H48), C50(H50), C51(H51), C52(H52), C53(H53),
 C54(H54), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60), C64(H64), C65(H65),
  C66(H66), C67(H67), C68(H68), C70(H70), C71(H71), C72(H72), C73(H73),
 C74(H74), C76(H76), C77(H77), C78(H78), C79(H79), C80(H80), C82(H82), C83(H83),
  C84(H84), C85(H85), C86(H86), C89(H89), C90(H90), C92(H92), C93(H93),
 C98(H98), C99(H99), C100(H100), C101(H101), C102(H102), C104(H104), C105(H105),
  C106(H106), C107(H107), C108(H108), C110(H110), C111(H111), C112(H112),
 C113(H113), C114(H114), C116(H116), C117(H117), C118(H118), C119(H119),
 C120(H120)
2.c Idealised Me refined as rotating group:
 C3A(H3AA,H3AB,H3AC), C4A(H4AA,H4AB,H4AC)
;
_shelx_res_checksum              25130
_shelx_hkl_checksum              71239
_shelx_fab_checksum              72554