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_7032047
_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         'C27 H35 Cl2 N3 O2 Pd, C H Cl3, 2(C2 H10 O)'
_chemical_formula_sum            'C32 H56 Cl5 N3 O4 Pd'
_chemical_formula_weight         830.44
_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-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7792(7)
_cell_length_b                   16.8591(9)
_cell_length_c                   17.8453(10)
_cell_measurement_reflns_used    3756
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21.03
_cell_measurement_theta_min      2.30
_cell_volume                     3844.7(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-2013 (Sheldrick, 2013)'
_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 0.994
_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  0.0717
_diffrn_reflns_av_unetI/netI     0.1006
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27200
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        26.300
_diffrn_reflns_theta_max         27.242
_diffrn_reflns_theta_min         1.662
_exptl_absorpt_coefficient_mu    0.868
_exptl_absorpt_correction_T_max  0.9043
_exptl_absorpt_correction_T_min  0.7715
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_description       prism
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.120
_platon_squeeze_details
;
 On the basis of synthetic conditions one can identify the disordered solvent
 present in the void.
 Since there are 342 electrons in the unit cell this gives 85.5 electrons per
 asymmetric unit and thus it is possible that this unit contains 2 molecules of
 diethyl ether (84 electrons). This gives 336 electrons per unit cell
 not too far away from the number of electrons estimated by
 PLATON SQUEEZE (342). The refinements without and with SQUEEZE treatment
 gave R1 factors of 9.49% and 6.59%, respectively. Therefore, the
 solvent-masking improved the results by 30.6%. 
 The disordered molecules were explicitly included into the CIF.
;
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.123
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.01(7)
_refine_ls_extinction_coef       0.0033(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         8552
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.1128
_refine_ls_R_factor_gt           0.0659
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0925P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1555
_refine_ls_wR_factor_ref         0.1744
_reflns_Friedel_coverage         0.803
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                4971
_reflns_number_total             8552
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt01917b2.cif
_cod_data_source_block           Compound11
_cod_depositor_comments
'Adding full bibliography for 7032046--7032050.cif.'
_cod_database_code               7032047
_shelx_estimated_absorpt_t_min   0.769
_shelx_estimated_absorpt_t_max   0.903
_shelxl_version_number           2014-3
_shelx_res_checksum              13768