Self-Assembled Cage Structures and Ethylene Polymerization Behavior of Palladium Alkyl Complexes That Contain Phosphine-Bis(arenesulfonate) Ligands
Wei, Jia; Shen, Zhongliang; Filatov, Alexander S.; Liu, Qian; Jordan, Richard F.; Organometallics 35 (2016) 3557–; doi:10.1021/acs.organomet.6b00629

data_4089008
_publ_section_title
;
 Self-Assembled Cage Structures and Ethylene Polymerization Behavior of
 Palladium Alkyl Complexes That Contain Phosphine-Bis(arenesulfonate)
 Ligands
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              3557
_journal_paper_doi               10.1021/acs.organomet.6b00629
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C120 H132 Li4 N4 O24 P4 Pd4 S8'
_chemical_formula_sum            'C120 H132 Li4 N4 O24 P4 Pd4 S8'
_chemical_formula_weight         2848.01
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary
;
dual-space method as implemented in SHELXT
;
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                73.353(3)
_cell_angle_beta                 78.196(3)
_cell_angle_gamma                82.657(3)
_cell_formula_units_Z            2
_cell_length_a                   17.7902(18)
_cell_length_b                   18.1177(18)
_cell_length_c                   26.642(3)
_cell_measurement_reflns_used    9614
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.01
_cell_measurement_theta_min      2.41
_cell_volume                     8031.3(15)
_computing_cell_refinement       'SAINT V.8.27 (Bruker AXS Inc., 2012)'
_computing_data_collection       'APEX2 v.2014.9-0 (Bruker AXS Inc., 2014)'
_computing_data_reduction        'SAINT V.8.27 (Bruker AXS Inc., 2012)'
_computing_molecular_graphics
;
Ortep-3 for Windows: L. J. Farrugia, J. Appl. Cryst (1997), 30, 565

Mercury: visualization and analysis of crystal structures
C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, 
R. Taylor, M. Towler and J. van de Streek, J. Appl. Cryst., 39, 453-457, 2006 
;
_computing_publication_material  'APEX2 v.2014.9-0 (Bruker AXS Inc., 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_source         'INCOATEC ImuS micro-focus source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            139234
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.081
_diffrn_reflns_theta_max         25.081
_diffrn_reflns_theta_min         2.015
_exptl_absorpt_coefficient_mu    0.639
_exptl_absorpt_correction_T_max  0.9701
_exptl_absorpt_correction_T_min  0.8374
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS (version 2012/4) as implemented in APEX2, version 2014.9-0, Bruker AXS
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_description       plate
_exptl_crystal_F_000             2912
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.961
_refine_diff_density_min         -1.297
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1633
_refine_ls_number_reflns         28459
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0661P)^2^+11.0926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1178
_refine_ls_wR_factor_ref         0.1306
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20623
_reflns_number_total             28459
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00629_si_002.cif
_cod_data_source_block           5b_jiawei0032
_cod_original_cell_volume        8031.4(14)
_cod_database_code               4089008
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.798
_shelx_estimated_absorpt_t_max   0.939
_shelx_res_checksum              2452
_shelx_hkl_checksum              16041
_shelx_fab_checksum              40753