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_4089009
_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         'C128 H148 Li4 N4 O24 P4 Pd4 S8'
_chemical_formula_sum            'C128 H148 Li4 N4 O24 P4 Pd4 S8'
_chemical_formula_weight         2960.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 99.758(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.2325(5)
_cell_length_b                   30.5438(8)
_cell_length_c                   29.0647(9)
_cell_measurement_reflns_used    9943
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50.47
_cell_measurement_theta_min      2.74
_cell_volume                     16826.6(8)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1568
_diffrn_reflns_av_unetI/netI     0.1945
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            53437
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        50.538
_diffrn_reflns_theta_max         50.538
_diffrn_reflns_theta_min         2.114
_exptl_absorpt_coefficient_mu    5.127
_exptl_absorpt_correction_T_max  0.750
_exptl_absorpt_correction_T_min  0.536
_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    1.169
_exptl_crystal_description       plate
_exptl_crystal_F_000             6080
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.869
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1613
_refine_ls_number_reflns         17475
_refine_ls_number_restraints     1665
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1784
_refine_ls_R_factor_gt           0.0945
_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^)+(0.1209P)^2^+6.5951P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2144
_refine_ls_wR_factor_ref         0.2498
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9039
_reflns_number_total             17475
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00629_si_002.cif
_cod_data_source_block           5d_jiawei0038
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4089009
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.328
_shelx_estimated_absorpt_t_max   0.715
_shelx_res_checksum              37208
_shelx_hkl_checksum              64574
_shelx_fab_checksum              92090