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_4089007
_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         'C152.50 H196 Li4 N4 O24 P4 Pd4 S8'
_chemical_formula_sum            'C152.5 H196 Li4 N4 O24 P4 Pd4 S8'
_chemical_formula_weight         3302.86
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   33.568(3)
_cell_length_b                   30.197(2)
_cell_length_c                   35.307(3)
_cell_measurement_reflns_used    9696
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.75
_cell_measurement_theta_min      2.22
_cell_volume                     35789(5)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0729
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            18836
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        20.891
_diffrn_reflns_theta_max         20.891
_diffrn_reflns_theta_min         2.025
_exptl_absorpt_coefficient_mu    0.583
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_description       block
_exptl_crystal_F_000             13720
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.250
_platon_squeeze_details
;
;
_refine_diff_density_max         1.451
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1559
_refine_ls_number_reflns         18836
_refine_ls_number_restraints     1828
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1191
_refine_ls_R_factor_gt           0.0994
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0637P)^2^+885.2977P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2374
_refine_ls_wR_factor_ref         0.2468
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14929
_reflns_number_total             18836
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00629_si_002.cif
_cod_data_source_block           4b_jiawei03
_cod_original_cell_volume        35790(5)
_cod_original_formula_sum        'C152.50 H196 Li4 N4 O24 P4 Pd4 S8'
_cod_database_code               4089007
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.854
_shelx_estimated_absorpt_t_max   0.868
_shelx_res_checksum              90250
_shelx_hkl_checksum              49793