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_4344225
_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         'C128 H112 P8 Pd4 S4, 4(C F3 O3 S)'
_chemical_formula_sum            'C132 H112 F12 O12 P8 Pd4 S8'
_chemical_formula_weight         3048.05
_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             2014-03-20
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                92.291(2)
_cell_angle_beta                 113.233(2)
_cell_angle_gamma                91.287(2)
_cell_formula_units_Z            1
_cell_length_a                   14.619(3)
_cell_length_b                   14.797(3)
_cell_length_c                   18.150(3)
_cell_measurement_reflns_used    9408
_cell_measurement_temperature    110.15
_cell_measurement_theta_max      27.529
_cell_measurement_theta_min      2.295
_cell_volume                     3601.8(12)
_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 0.993
_diffrn_measured_fraction_theta_max 0.969
_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  0.0280
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            40761
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.550
_diffrn_reflns_theta_min         1.891
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.766
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6366
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0501 before and 0.0387 after correction.
The Ratio of minimum to maximum transmission is 0.8538.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_description       block
_exptl_crystal_F_000             1540
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.15
_refine_diff_density_max         3.049
_refine_diff_density_min         -1.179
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     939
_refine_ls_number_reflns         16120
_refine_ls_number_restraints     516
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0466
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0737P)^2^+7.5037P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1257
_refine_ls_wR_factor_ref         0.1359
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13396
_reflns_number_total             16120
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00806_si_002.cif
_cod_data_source_block           sd42_sq
_cod_depositor_comments
'Adding full bibliography for 4344224--4344226.cif.'
_cod_original_cell_volume        3601.6(11)
_cod_database_code               4344225
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.894
_shelx_estimated_absorpt_t_min   0.826
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
 S1C, S1D, O2C, O3C, O4C, C5C, F6C, F7C, F8C, O2D, O3D, O4D, C5D, F6D, F7D, F8D
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 S9C, S9D, O10C, O11C, O12C, C13C, F14C, F15C, F16C, O10D, O11D, O12D, C13D,
 F14D, F15D, F16D
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
S1C \\sim S1D \\sim O2C \\sim O3C \\sim O4C \\sim C5C \\sim F6C \\sim F7C \\sim
F8C \\sim O2D \\sim O3D \\sim O4D \\sim C5D \\sim F6D \\sim F7D \\sim F8D:
within 1.7A with sigma of 0.005 and sigma for terminal atoms of 0.01
S9C \\sim S9D \\sim O10C \\sim O11C \\sim O12C \\sim C13C \\sim F14C \\sim F15C
\\sim F16C \\sim O10D \\sim O11D \\sim O12D \\sim C13D \\sim F14D \\sim F15D
\\sim F16D: within 1.7A with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Same fragment restrains
{S1C, O2C, O3C, O4C, C5C, F6C, F7C, F8C}
as
{S1D, O2D, O3D, O4D, C5D, F6D, F7D, F8D}
{S9C, O10C, O11C, O12C, C13C, F14C, F15C, F16C}
as
{S9D, O10D, O11D, O12D, C13D, F14D, F15D, F16D}
5. Others
 Sof(S1D)=Sof(O2D)=Sof(O3D)=Sof(O4D)=Sof(C5D)=Sof(F6D)=Sof(F7D)=Sof(F8D)=1-
 FVAR(1)
 Sof(S1C)=Sof(O2C)=Sof(O3C)=Sof(O4C)=Sof(C5C)=Sof(F6C)=Sof(F7C)=Sof(F8C)=FVAR(1)
 Sof(S9D)=Sof(O10D)=Sof(O11D)=Sof(O12D)=Sof(C13D)=Sof(F14D)=Sof(F15D)=
 Sof(F16D)=1-FVAR(2)
 Sof(S9C)=Sof(O10C)=Sof(O11C)=Sof(O12C)=Sof(C13C)=Sof(F14C)=Sof(F15C)=
 Sof(F16C)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C39(H39A,H39B), C40(H40A,H40B)
6.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), C28(H28), C29(H29), C31(H31),
 C32(H32), C34(H34), C35(H35), C37(H37), C38(H38), C42(H42), C43(H43), C44(H44),
  C45(H45), C46(H46), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52),
 C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C60(H60), C61(H61), C62(H62),
  C63(H63), C64(H64)
;
_shelx_res_checksum              84808
_shelx_hkl_checksum              46435
_shelx_fab_checksum              5693