Synthesis and structural characterization of 20-membered macrocyclic rings bearing trans-chelating bis(N-heterocyclic carbene) ligands and the catalytic activity of their palladium(ii) complexes.
Thapa, Rajesh; Kilyanek, Stefan M.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 12577–12590; doi:10.1039/c9dt02147g

data_7700626
_publ_section_title
;
 Synthesis and structural characterization of 20-membered macrocyclic
 rings bearing trans-chelating bis(N-heterocyclic carbene) ligands and the
 catalytic activity of their palladium(ii) complexes.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12577
_journal_page_last               12590
_journal_paper_doi               10.1039/c9dt02147g
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety
'0.57(C40 H46 Cl2 N6 Pd), 0.43(C40 H46 Br Cl N6 Pd)'
_chemical_formula_sum            'C40 H46 Br0.43 Cl1.57 N6 Pd'
_chemical_formula_weight         807.24
_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-06-29 deposited with the CCDC.    2019-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.665(19)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.462(17)
_cell_length_b                   10.751(15)
_cell_length_c                   14.335(19)
_cell_measurement_reflns_used    2452
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.24
_cell_measurement_theta_min      2.39
_cell_volume                     1866(4)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX3 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'Mercury (CCDC, 2017)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2015b)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1061
_diffrn_reflns_av_unetI/netI     0.0682
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14735
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        22.722
_diffrn_reflns_theta_max         22.722
_diffrn_reflns_theta_min         1.950
_exptl_absorpt_coefficient_mu    1.107
_exptl_absorpt_correction_T_max  0.3782
_exptl_absorpt_correction_T_min  0.2597
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/4 (Sheldrick, 2015c)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_description       block
_exptl_crystal_F_000             831
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.779
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         2508
_refine_ls_number_restraints     667
_refine_ls_restrained_S_all      0.903
_refine_ls_R_factor_all          0.1106
_refine_ls_R_factor_gt           0.0879
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1400P)^2^+20.3000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2480
_refine_ls_wR_factor_ref         0.2636
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1897
_reflns_number_total             2508
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02147g2.cif
_cod_data_source_block           17191a
_cod_depositor_comments
'Adding full bibliography for 7700623--7700627.cif.'
_cod_database_code               7700626
_shelx_estimated_absorpt_t_min   0.660
_shelx_estimated_absorpt_t_max   0.907
_shelx_res_checksum              15007