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_4089010
_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_sum            'C119.5 H182 Cl5 Li3 N3 O18 P3 Pd3 S6'
_chemical_formula_weight         2751.21
_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
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                75.162(3)
_cell_angle_beta                 72.865(3)
_cell_angle_gamma                82.851(3)
_cell_formula_units_Z            2
_cell_length_a                   18.991(2)
_cell_length_b                   19.582(2)
_cell_length_c                   23.263(3)
_cell_measurement_reflns_used    9404
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.98
_cell_measurement_theta_min      2.28
_cell_volume                     7980.2(16)
_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 0.999
_diffrn_measured_fraction_theta_max 0.991
_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  0.0415
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            201245
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.052
_diffrn_reflns_theta_min         2.143
_exptl_absorpt_coefficient_mu    0.577
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.609
_exptl_absorpt_correction_type   multi-scan
_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    1.145
_exptl_crystal_description       block
_exptl_crystal_F_000             2874
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.120
_refine_diff_density_max         3.948
_refine_diff_density_min         -1.637
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1481
_refine_ls_number_reflns         34714
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0564
_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^)+(0.0859P)^2^+21.6112P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1511
_refine_ls_wR_factor_ref         0.1669
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27052
_reflns_number_total             34714
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00629_si_002.cif
_cod_data_source_block           6e_jiawei08
_cod_original_cell_volume        7980.0(15)
_cod_original_formula_sum        'C119.50 H182 Cl5 Li3 N3 O18 P3 Pd3 S6'
_cod_database_code               4089010
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.855
_shelx_estimated_absorpt_t_max   0.934
_shelx_res_checksum              90234
_shelx_hkl_checksum              25422
_shelx_fab_checksum              24491