Synthesis, Structures, and Norbornene Polymerization Behavior of N-Heterocyclic Carbene-Sulfonate-Ligated Palladacycles
Li, Minliang; Song, Haibin; Wang, Baiquan; Organometallics 34 (2015) 1969–; doi:10.1021/acs.organomet.5b00214

data_4085743
_publ_section_title
;
 Synthesis, Structures, and Norbornene Polymerization Behavior of
 N-Heterocyclic Carbene-Sulfonate-Ligated Palladacycles
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              1969
_journal_paper_doi               10.1021/acs.organomet.5b00214
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C31 H31 Cl2 N3 O3 Pd S'
_chemical_formula_sum            'C31 H31 Cl2 N3 O3 Pd S'
_chemical_formula_weight         702.95
_chemical_name_systematic
; 
 ? 
;
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 98.494(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9780(14)
_cell_length_b                   11.1650(12)
_cell_length_c                   17.977(2)
_cell_measurement_reflns_used    16002
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      36.30
_cell_measurement_theta_min      1.40
_cell_volume                     2973.3(5)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r4'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r4'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2009)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 14.222
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku Saturn724 CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0595
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            57380
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.275
_diffrn_reflns_theta_min         1.654
_exptl_absorpt_coefficient_mu    0.912
_exptl_absorpt_correction_T_max  0.833
_exptl_absorpt_correction_T_min  0.663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.892
_refine_diff_density_min         -1.455
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         14285
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0388P)^2^+0.4554P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.0936
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12603
_reflns_number_total             14285
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00214_si_001.cif
_cod_data_source_block           6d
_cod_depositor_comments
'Adding full bibliography for 4085742--4085745.cif.'
_cod_database_code               4085743
_shelx_estimated_absorpt_t_min   0.797
_shelx_estimated_absorpt_t_max   0.839
_shelxl_version_number           2013-3
_shelx_res_checksum              93291
_shelx_hkl_checksum              93764