Phenylene- and Biphenylene-Bridged Bis-Imidazolylidenes of Palladium. Influence of the Presence of Pyrene Tags on the Catalytic Activity of the Complexes
Ruiz-Botella, Sheila; Peris, Eduardo; Organometallics 33 (2014) 5509–; doi:10.1021/om500765u

data_4084738
_publ_section_title
;
 Phenylene- and Biphenylene-Bridged Bis-Imidazolylidenes of Palladium.
 Influence of the Presence of Pyrene Tags on the Catalytic Activity of the
 Complexes
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5509
_journal_paper_doi               10.1021/om500765u
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety
'C64 H46 Br4 Cl2 N6 Pd2, 4(C H Cl3), 2(C H-0.5 Cl2.75)'
_chemical_formula_sum            'C70 H49 Br4 Cl19.5 N6 Pd2'
_chemical_formula_weight         2197.86
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2014-07-17
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_cell_angle_alpha                64.449(2)
_cell_angle_beta                 61.369(2)
_cell_angle_gamma                62.9117(19)
_cell_formula_units_Z            1
_cell_length_a                   13.8715(3)
_cell_length_b                   13.9886(3)
_cell_length_c                   14.2318(3)
_cell_measurement_temperature    220
_cell_volume                     2076.21(9)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      220
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            41128
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.989
_diffrn_reflns_theta_min         2.843
_exptl_absorpt_coefficient_mu    3.029
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.638
_exptl_absorpt_correction_type   gaussian
_exptl_crystal_colour            yellowish
_exptl_crystal_density_diffrn    1.758
_exptl_crystal_F_000             1074
_exptl_crystal_size_max          0.475
_exptl_crystal_size_mid          0.286
_exptl_crystal_size_min          0.135
_refine_diff_density_max         2.483
_refine_diff_density_min         -1.927
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         8149
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_gt           0.0807
_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^)+(0.1670P)^2^+10.4990P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2536
_refine_ls_wR_factor_ref         0.2849
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6238
_reflns_number_total             8149
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500765u_si_001.cif
_cod_data_source_block           str1634(1)
_cod_original_cell_volume        2076.20(9)
_cod_original_formula_sum        'C70 H49 Br4 Cl19.50 N6 Pd2'
_cod_database_code               4084738
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Fixed Sof: H1A(-0.5) Cl2(0.75) Cl3(0.25) Cl11(0.75)
3.a Ternary CH refined with riding coordinates:
 C34(H34), C1A(H1A), C35(H35)
3.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C7(H7), C8(H8), C10(H10), C11(H11), C14(H14), C15(H15),
 C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C24(H24), C25(H25), C28(H28),
  C30(H30), C31(H31), C32(H32)
;
_shelx_res_checksum              22531
_shelx_hkl_checksum              31677
_olex2_submission_special_instructions 'No special instructions were received'