Trimethyl-palladium(IV) and -platinum(IV) complexes containing phosphine donor ligands, including studies of 1,5,9-triethyl-1,5,9-triphosphacyclodecane and X-ray structural studies of palladium(II) and palladium(IV) complexes †
Bayler, Angela; Canty, Allan J.; Edwards, Peter G.; Skelton, Brian W.; White, Allan H.; Journal of the Chemical Society, Dalton Transactions  (2000) 3325–; doi:10.1039/b004741o

data_7009952
_publ_section_title
;
 Trimethyl-palladium(IV) and -platinum(IV) complexes containing
 phosphine donor ligands, including studies of
 1,5,9-triethyl-1,5,9-triphosphacyclodecane and X-ray structural
 studies of palladium(II) and palladium(IV) complexes&#x200A;&#x2020;
;
_journal_issue                   19
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3325
_journal_paper_doi               10.1039/b004741o
_journal_year                    2000
_chemical_formula_sum            'C20 H22 F3 N2 O3 P Pd S'
_chemical_formula_weight         564.86
_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'
_cell_angle_alpha                90.00000
_cell_angle_beta                 98.6520(10)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            4
_cell_length_a                   9.6042(9)
_cell_length_b                   11.5323(10)
_cell_length_c                   20.241(2)
_cell_measurement_reflns_used    7834
_cell_measurement_temperature    150
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     2216.4(4)
_computing_cell_refinement       'Siemens SAINT (Siemens, 1995)'
_computing_data_collection       'Siemens SMART (Siemens, 1995)'
_computing_data_reduction        'xtal ADDREF SORTRF'
_computing_molecular_graphics    xtal
_computing_publication_material  'xtal BONDLA CIFIO'
_computing_structure_refinement  'xtal CRYLSQ'
_computing_structure_solution    xtal
_diffrn_ambient_temperature      150
_diffrn_measurement_device_type
;
Bruker SMART CCD diffractometer
;
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_detector       'CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0274
_diffrn_reflns_av_sigmaI/netI    .045
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            21967
_diffrn_reflns_theta_max         29.08
_diffrn_reflns_theta_min         2.04
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.053
_exptl_absorpt_correction_T_max  .831
_exptl_absorpt_correction_T_min  .714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS; Sheldrick, 1996
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_description       prism
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          .25
_exptl_crystal_size_mid          .15
_exptl_crystal_size_min          .13
_refine_diff_density_max         .99
_refine_diff_density_min         -.625
_refine_ls_goodness_of_fit_all   1.099
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     368
_refine_ls_number_reflns         4590
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .041
_refine_ls_R_factor_gt           .03
_refine_ls_shift/su_max          .038
_refine_ls_shift/su_mean         .001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .037
_refine_ls_wR_factor_ref         .035
_reflns_d_resolution_high        .731
_reflns_d_resolution_low         9.985
_reflns_Friedel_coverage         0
_reflns_limit_h_max              12
_reflns_limit_h_min              0
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              -27
_reflns_number_gt                4590
_reflns_number_total             5635
_reflns_threshold_expression     'F    > 4.00 sig(F   )'
_cod_data_source_file            b004741o.txt
_cod_data_source_block           pdabgn
_cod_original_sg_symbol_Hall     -p_2yn
_cod_original_sg_symbol_H-M      P_1_21/n_1
_cod_original_formula_sum        'C20 H22 F3 N2 O3 P1 Pd1 S1'
_cod_database_code               7009952