Thiocarbarmoyl-Assisted Formation of a New Type of α- and β-Isomer Paddlewheel Pd24+Compounds. Synthesis, Characterization, and Crystal Structures of [Pd(η1-SCNMe2)(η2-Tp)(PPh3)], [Pd2(μ-Hdppa)2(μ-SCNMe2)2][Cl]2, [Pd2(μ-dppa)2(μ-SCNMe2)2], and [Pd{η2-S2P(OEt)2}]2(μ-dppa)(μ-SCNMe2)
Yih, Kuang-Hway; Lee, Gene-Hsiang; Organometallics 29 (2010) 3397–; doi:10.1021/om100558m

data_4066648
_publ_section_title
;
 Thiocarbarmoyl-Assisted Formation of a New Type of \a- and \b-Isomer
 Paddlewheel Pd24+Compounds. Synthesis, Characterization, and Crystal
 Structures of [Pd(\h1-SCNMe2)(\h2-Tp)(PPh3)],
 [Pd2(\m-Hdppa)2(\m-SCNMe2)2][Cl]2, [Pd2(\m-dppa)2(\m-SCNMe2)2], and
 [Pd{\h2-S2P(OEt)2}]2(\m-dppa)(\m-SCNMe2)
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3397
_journal_paper_doi               10.1021/om100558m
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C62 H66 Cl2 N8 P4 Pd2 S2'
_chemical_formula_weight         1394.93
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.5167(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.6065(1)
_cell_length_b                   17.0851(2)
_cell_length_c                   13.9854(2)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.87
_cell_volume                     3147.37(6)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'NONIUS COLLECT'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(1)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0758
_diffrn_reflns_av_sigmaI/netI    0.0802
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22929
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.870
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.590
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.069
_refine_diff_density_min         -1.303
_refine_diff_density_rms         0.262
_refine_ls_extinction_coef       0.0123(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         7223
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0738P)^2^+0.3751P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1167
_refine_ls_wR_factor_ref         0.1402
_reflns_number_gt                5053
_reflns_number_total             7223
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100558m_si_001.cif
_cod_data_source_block           ic9105
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4066648