Structural Modification of Functionalized Phosphine Sulfonate-Based Palladium(II) Olefin Polymerization Catalysts
Anselment, Timo M. J.; Wichmann, Christian; Anderson, Carly E.; Herdtweck, Eberhardt; Rieger, Bernhard; Organometallics 30 (2011) 6602–; doi:10.1021/om200734x

data_4065370
_publ_section_title
;
 Structural Modification of Functionalized Phosphine Sulfonate-Based
 Palladium(II) Olefin Polymerization Catalysts
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              6602
_journal_paper_doi               10.1021/om200734x
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C64 H66 N2 O10 P2 Pd2 S2, C H Cl3'
_chemical_formula_sum            'C65 H67 Cl3 N2 O10 P2 Pd2 S2'
_chemical_formula_weight         1481.44
_chemical_name_systematic        ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 110.6878(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.1506(9)
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_cell_length_c                   24.5348(9)
_cell_measurement_reflns_used    9272
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      25.46
_cell_measurement_theta_min      1.64
_cell_volume                     7827.7(5)
_computing_cell_refinement       'SAINT (Bruker, 2008b)'
_computing_data_collection       'APEX II Control Software (Bruker, 2008a)'
_computing_data_reduction        'SAINT (Bruker, 2008b)'
_computing_molecular_graphics    'PLATON (Spek, 2010)'
_computing_publication_material  'PLATON (Spek, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1998)'
_computing_structure_solution    'SIR92 (Altomare, 1994)'
_diffrn_ambient_temperature      123(1)
_diffrn_detector                 ' CCD plate '
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       ' \k-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker APEX-II CCD '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0117
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_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
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_diffrn_reflns_theta_full        25.46
_diffrn_reflns_theta_max         25.46
_diffrn_reflns_theta_min         1.64
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.705
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6507
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker, 2008b'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       fragment
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_exptl_crystal_size_max          0.46
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_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.648
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_reflns         14451
_refine_ls_number_restraints     0
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_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0344
_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^)+(0.0465P)^2^+10.7405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.0935
_reflns_number_gt                13066
_reflns_number_total             14451
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om200734x_si_002.cif
_cod_data_source_block           Compound_10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4065370