Hemilabile bonding of 1-oxa-4,7-dithiacyclononane in cyclometallated palladium(ii) complexes.
Janzen, Daron E.; Bruening, Meaghan A.; Mamiya, Arthur A.; Driscoll, Laura E.; da Silva Filho, Demetrio A.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 11520–11535; doi:10.1039/c9dt02059d

data_7700403
_publ_section_title
;
 Hemilabile bonding of 1-oxa-4,7-dithiacyclononane in cyclometallated
 palladium(ii) complexes.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11520
_journal_page_last               11535
_journal_paper_doi               10.1039/c9dt02059d
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C18 H20 N O2 Pd S2, F6 P'
_chemical_formula_sum            'C18 H20 F6 N O2 P Pd S2'
_chemical_formula_weight         597.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2019-02-01 deposited with the CCDC.    2019-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 114.020(8)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   14.3588(14)
_cell_length_b                   12.2238(13)
_cell_length_c                   13.3861(14)
_cell_measurement_reflns_used    17509
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.64
_cell_measurement_theta_min      3.05
_cell_volume                     2146.1(4)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r13'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r13'
_computing_molecular_graphics    'CrystalStructure 4.1'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean 6.849
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku XtaLAB mini'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_unetI/netI     0.070
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21879
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         3.050
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.202
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.638
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.850
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1192.00
_exptl_crystal_size_max          0.800
_exptl_crystal_size_mid          0.330
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.76
_refine_diff_density_min         -0.64
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     302
_refine_ls_number_reflns         4926
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0473
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0510P)^2^+3.0557P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1170
_reflns_number_gt                3731
_reflns_number_total             4926
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c9dt02059d2.cif
_cod_data_source_block           2b
_cod_depositor_comments
'Adding full bibliography for 7700398--7700405.cif.'
_cod_database_code               7700403
_shelxl_version_number           2013-3
_shelx_res_checksum              36854