Catalytic asymmetric hydrogenation using [2.2]paracyclophane based chiral 1,2,3-triazol-5-ylidene-Pd complex under ambient conditions and 1 atmosphere of H2
Sankararaman, Sethuraman; V, Ramkumar; Dasgupta, Ayan; RSC Adv.  (2015) –; doi:10.1039/C5RA03021H

data_7219595
_publ_section_title
;
 Catalytic asymmetric hydrogenation using [2.2]paracyclophane based chiral
 1,2,3-triazol-5-ylidene-Pd complex under ambient conditions and 1
 atmosphere of H2
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA03021H
_journal_year                    2015
_chemical_formula_sum            'C28 H28 Cl2 N4 Pd'
_chemical_formula_weight         597.84
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2014-04-28 deposited with the CCDC.
2015-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.6305(2)
_cell_length_b                   15.1575(3)
_cell_length_c                   22.3524(5)
_cell_measurement_temperature    296(2)
_cell_volume                     2585.26(10)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0152
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12095
_diffrn_reflns_point_group_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         1.623
_exptl_absorpt_coefficient_mu    0.949
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.186
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details
;
 Flack x determined using 1789 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.008(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         4465
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0194
_refine_ls_R_factor_gt           0.0182
_refine_ls_shift/su_max          0.063
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0161P)^2^+0.9707P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0428
_refine_ls_wR_factor_ref         0.0435
_reflns_Friedel_coverage         0.715
_reflns_Friedel_fraction_full    0.932
_reflns_Friedel_fraction_max     0.961
_reflns_number_gt                4329
_reflns_number_total             4465
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra03021h2.cif
_cod_data_source_block           acn
_cod_database_code               7219595
_shelx_estimated_absorpt_t_min   0.797
_shelx_estimated_absorpt_t_max   0.871
_shelxl_version_number           2013-4
_shelx_res_checksum              60732
_shelx_hkl_checksum              45933