New, potentially chelating NHC ligands; synthesis, complexation studies, and preliminary catalytic evaluation.
Ou, Arnold; Wu, Linglin; Salvador, Alvaro; Sipos, Gellert; Zhao, Guangzhen; Skelton, Brian W.; Sobolev, Alexandre N.; Dorta, Reto; Dalton transactions (Cambridge, England : 2003) 46 (2017) 3631–3641; doi:10.1039/c6dt04534k

data_7042172
_publ_section_title
;
 New, potentially chelating NHC ligands; synthesis, complexation studies,
 and preliminary catalytic evaluation.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3631
_journal_page_last               3641
_journal_paper_doi               10.1039/c6dt04534k
_journal_volume                  46
_journal_year                    2017
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C42 H45 Cl N4 Pd'
_chemical_formula_sum            'C42 H45 Cl N4 Pd'
_chemical_formula_weight         747.67
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      43
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-03-15T11:27:10-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2016-11-24 deposited with the CCDC.
2017-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            32
_cell_length_a                   86.5994(8)
_cell_length_b                   25.6783(3)
_cell_length_c                   12.9003(2)
_cell_measurement_reflns_used    21809
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.612
_cell_measurement_theta_min      1.841
_cell_volume                     28686.7(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Diamond (Brandenburg, K., (1999)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0009
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0077591
_diffrn_orient_matrix_UB_12      -0.008674
_diffrn_orient_matrix_UB_13      -0.0031896
_diffrn_orient_matrix_UB_21      -0.0025527
_diffrn_orient_matrix_UB_22      0.0262191
_diffrn_orient_matrix_UB_23      -0.0028287
_diffrn_orient_matrix_UB_31      0.00059
_diffrn_orient_matrix_UB_32      -0.0008261
_diffrn_orient_matrix_UB_33      -0.0548118
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_av_unetI/netI     0.0723
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       106
_diffrn_reflns_limit_h_min       -124
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            77123
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        30
_diffrn_reflns_theta_max         31.414
_diffrn_reflns_theta_min         1.902
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.628
_exptl_absorpt_correction_T_max  0.956
_exptl_absorpt_correction_T_min  0.808
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
       CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_description       plate
_exptl_crystal_F_000             12416
_exptl_crystal_size_max          0.581
_exptl_crystal_size_mid          0.233
_exptl_crystal_size_min          0.072
_refine_diff_density_max         2.095
_refine_diff_density_min         -1.275
_refine_diff_density_rms         0.116
_refine_ls_abs_structure_details
;
 Flack x determined using 8117 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.038(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         22322
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.192
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0651
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+258.6184P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.145
_refine_ls_wR_factor_ref         0.147
_reflns_number_gt                21032
_reflns_number_total             22322
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04534k2.cif
_cod_data_source_block           rda606o
_cod_depositor_comments
'Adding full bibliography for 7042167--7042177.cif.'
_cod_database_code               7042172
_shelx_res_checksum              90988