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_4344224
_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
'C116 H104 P8 Pd4 S4, 4(C F3 O3 S), 0.36(C H2 Cl2)'
_chemical_formula_sum            'C120.36 H104.72 Cl0.72 F12 O12 P8 Pd4 S8'
_chemical_formula_weight         2926.61
_chemical_name_systematic
;
 ?
;
_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             2014-03-26
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                79.209(2)
_cell_angle_beta                 85.456(2)
_cell_angle_gamma                70.708(2)
_cell_formula_units_Z            1
_cell_length_a                   13.145(2)
_cell_length_b                   14.789(3)
_cell_length_c                   16.778(3)
_cell_measurement_reflns_used    9764
_cell_measurement_temperature    110.15
_cell_measurement_theta_max      27.329
_cell_measurement_theta_min      2.357
_cell_volume                     3023.5(9)
_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 0.996
_diffrn_measured_fraction_theta_max 0.979
_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  0.0222
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_laue_measured_fraction_full 0.996
_diffrn_reflns_laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34721
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.414
_diffrn_reflns_theta_min         1.759
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.924
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0446 before and 0.0343 after correction.
The Ratio of minimum to maximum transmission is 0.9126.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_description       block
_exptl_crystal_F_000             1475
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     766
_refine_ls_number_reflns         13475
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0270
_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^)+(0.0257P)^2^+2.3129P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0600
_refine_ls_wR_factor_ref         0.0639
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11760
_reflns_number_total             13475
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00806_si_002.cif
_cod_data_source_block           sd37rb
_cod_depositor_comments
'Adding full bibliography for 4344224--4344226.cif.'
_cod_original_cell_volume        3023.6(10)
_cod_database_code               4344224
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.830
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Fixed Sof: Cl1S(0.181) Cl2S(0.181) C1S(0.181) H1SA(0.181) H1SB(0.181)
3.a Secondary CH2 refined with riding coordinates:
 C1(H,HA), C2(HB,HC), C27(HX,HY), C28(HZ,H0AA), C1S(H1SA,H1SB)
3.b Aromatic/amide H refined with riding coordinates:
 C4(HD), C5(HE), C6(HF), C7(HG), C8(HH), C10(HI), C11(HJ), C12(HK), C13(HL),
 C14(HM), C16(HN), C17(HO), C18(HP), C19(HQ), C20(HR), C22(HS), C23(HT),
 C24(HU), C25(HV), C26(HW), C30(H1AA), C31(H2AA), C32(H3AA), C33(H4AA),
 C34(H5AA), C36(H6AA), C37(H7AA), C38(H8AA), C39(H9AA), C40(H0BA), C42(H1BA),
 C43(H2BA), C44(H3BA), C45(H4BA), C46(H5BA), C48(H6BA), C49(H7BA), C50(H8BA),
 C51(H9BA), C52(H0CA), C54(H1CA), C55(H2CA), C57(H3CA), C58(H4CA)
;
_shelx_res_checksum              16597
_shelx_hkl_checksum              77370