Metal-mediated coupling of amino acid esters with isocyanides leading to new chiral acyclic aminocarbene complexes.
Anisimova, Tatyana B.; Guedes da Silva, M Fátima C; Kukushkin, Vadim Yu; Pombeiro, Armando J. L.; Luzyanin, Konstantin V.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 15861–15871; doi:10.1039/c4dt01917b

data_7032046
_publ_section_title
;
 Metal-mediated coupling of amino acid esters with isocyanides leading to
 new chiral acyclic aminocarbene complexes.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15861
_journal_page_last               15871
_journal_paper_doi               10.1039/c4dt01917b
_journal_volume                  43
_journal_year                    2014
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C28 H31 Cl2 N3 O3 Pd'
_chemical_formula_sum            'C28 H31 Cl2 N3 O3 Pd'
_chemical_formula_weight         634.86
_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
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.3881(4)
_cell_length_b                   17.1311(6)
_cell_length_c                   26.0983(10)
_cell_measurement_reflns_used    9911
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.04
_cell_measurement_theta_min      2.42
_cell_volume                     6432.8(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0621
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            40590
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         27.148
_diffrn_reflns_theta_min         1.422
_exptl_absorpt_coefficient_mu    0.773
_exptl_absorpt_correction_T_max  0.8484
_exptl_absorpt_correction_T_min  0.7683
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_description       prism
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.220
_platon_squeeze_details
;
 It was not possible to unambiguously identify the disordered solvent(s).
 Since there are 484 electrons in all which gives 60.8 electrons per
 asymmetric unit, it is possible that this unit contains 1 molecule of
 chloroform (58 electrons) or 1 molecule of isopropyl ether (also, 58
 electrons). This gives 464 electrons, not too far away from the number
 of electrons estimated by PLATON SQUEEZE. The refinements without and
 with SQUEEZE treatment gave R1 factors of 13.51% and 4.39%, respectively,
 and thus the solvent-masking improved the result by 67.5%. 
 The doubt in identifying the disordered molecules prevented their
 explicit inclusion into the CIF.
;
_refine_diff_density_max         1.065
_refine_diff_density_min         -0.879
_refine_diff_density_rms         0.189
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.03(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.684
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     669
_refine_ls_number_reflns         13994
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.684
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0439
_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^)+(0.1671P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1335
_refine_ls_wR_factor_ref         0.1447
_reflns_Friedel_coverage         0.829
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                11853
_reflns_number_total             13994
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt01917b2.cif
_cod_data_source_block           Compound9
_cod_depositor_comments
'Adding full bibliography for 7032046--7032050.cif.'
_cod_database_code               7032046
_shelx_estimated_absorpt_t_min   0.768
_shelx_estimated_absorpt_t_max   0.848
_shelxl_version_number           2013-4
_shelx_res_checksum              3647