Bis(imino)acenaphthene (BIAN)-supported palladium(ii) carbene complexes as effective C‒C coupling catalysts and solvent effects in organic and aqueous media
Crawford, Katherine A.; Cowley, Alan H.; Humphrey, Simon M.; Catalysis Science & Technology 4 (2014) 1456–; doi:10.1039/c4cy00192c

data_1514273
_publ_section_title
;
 Bis(imino)acenaphthene (BIAN)-supported palladium(ii) carbene complexes
 as effective C--C coupling catalysts and solvent effects in organic and
 aqueous media
;
_journal_issue                   5
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              1456
_journal_paper_doi               10.1039/c4cy00192c
_journal_volume                  4
_journal_year                    2014
_chemical_formula_moiety         C55H55Cl2N2P1Pd1
_chemical_formula_sum            'C55 H55 Cl2 N2 P Pd'
_chemical_formula_weight         952.28
_chemical_name_common            palladium(II)carbene
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90.014(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.669(4)
_cell_length_b                   12.248(4)
_cell_length_c                   31.450(10)
_cell_measurement_temperature    100(2)
_cell_volume                     4880(3)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0999
_diffrn_reflns_av_unetI/netI     0.0811
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            73165
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.607
_exptl_absorpt_coefficient_mu    0.560
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.799
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.28(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.288
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1116
_refine_ls_number_reflns         17136
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.286
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0767
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0399P)^2^+7.4286P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1611
_refine_ls_wR_factor_ref         0.1644
_reflns_Friedel_coverage         0.903
_reflns_Friedel_fraction_full    0.973
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                15954
_reflns_number_total             17136
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cy00192c2.cif
_cod_data_source_block           shelx
_cod_database_code               1514273
_shelx_estimated_absorpt_t_min   0.891
_shelx_estimated_absorpt_t_max   0.941
_shelxl_version_number           2013-4
_shelx_res_checksum              12422