Fluxional interconversion of divalent palladium complexes having NSNSN ligands between flexible SNS and rigid NNN-coordinated structures.
Kawada, Yumi; Kataoka, Yasutaka; Ura, Yasuyuki; Dalton transactions (Cambridge, England : 2003) 42 (2013) 14844–14855; doi:10.1039/c3dt51592c

data_7023623
_publ_section_title
;
 Fluxional interconversion of divalent palladium complexes having NSNSN
 ligands between flexible SNS and rigid NNN-coordinated structures.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14844
_journal_page_last               14855
_journal_paper_doi               10.1039/c3dt51592c
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C33 H28 N5 P Pd S2, C2 F6 O6 S2'
_chemical_formula_sum            'C35 H28 F6 N5 O6 P Pd S4'
_chemical_formula_weight         994.23
_chemical_melting_point_gt       478
_chemical_name_common            '[Pd(PSMePy)(PPh3)](OTf)2'
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/a 1'
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 110.727(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.7910(13)
_cell_length_b                   12.9731(6)
_cell_length_c                   18.4171(11)
_cell_measurement_reflns_used    30328
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.483
_cell_measurement_theta_min      3.073
_cell_volume                     3975.6(4)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    Ortep-III
_computing_publication_material  Ortep-III
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Rigaku Saturn724+ (4x4 bin mode)'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30328
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         3.073
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.797
_exptl_absorpt_correction_T_max  0.8569
_exptl_absorpt_correction_T_min  0.7960
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_transmission_factor_max   0.8569
_exptl_transmission_factor_min   0.7960
_refine_diff_density_max         0.861
_refine_diff_density_min         -1.214
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     540
_refine_ls_number_reflns         8934
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0535
_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^)+(0.0684P)^2^+4.1565P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1379
_refine_ls_wR_factor_ref         0.1493
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7329
_reflns_number_total             8934
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt51592c.txt
_cod_data_source_block           complex4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_melting_point_gt' since the value was specified 'more
than' ('>') a certain temperature. The value '>478' was changed to
'478' - it should be numeric and without a unit
designator.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_database_code               7023623
_shelx_estimated_absorpt_t_min   0.796
_shelx_estimated_absorpt_t_max   0.857
_shelxl_version_number           2013-4
_shelx_res_checksum              57273
_shelx_hkl_checksum              23511