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_7700627
_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         'C32 H44 N6, 2(C H Cl3), 2(Br)'
_chemical_formula_sum            'C34 H46 Br2 Cl6 N6'
_chemical_formula_weight         911.29
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-07-18 deposited with the CCDC.    2019-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_c                   25.649(8)
_cell_measurement_reflns_used    2245
_cell_measurement_temperature    100(2)
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_cell_measurement_theta_min      2.43
_cell_volume                     4028(2)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
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_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015b)'
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_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
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_diffrn_reflns_point_group_measured_fraction_full 1.000
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_exptl_absorpt_process_details   'TWINABS 2012/1 (Sheldrick, 2015c)'
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_exptl_crystal_description       block
_exptl_crystal_F_000             1856
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_exptl_crystal_size_min          0.110
_refine_diff_density_max         3.282
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0597
_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^)+(0.1150P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1605
_refine_ls_wR_factor_ref         0.1750
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7787
_reflns_number_total             11335
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_depositor_comments
'Adding full bibliography for 7700623--7700627.cif.'
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