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_7032048
_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         'C25 H29 Cl4 N3 O2 Pd, C H Cl3'
_chemical_formula_sum            'C26 H30 Cl7 N3 O2 Pd'
_chemical_formula_weight         771.08
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 104.4940(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.1788(6)
_cell_length_b                   12.3145(4)
_cell_length_c                   24.9100(6)
_cell_measurement_reflns_used    9973
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.16
_cell_measurement_theta_min      2.61
_cell_volume                     7180.9(3)
_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 0.808
_diffrn_measured_fraction_theta_max 0.996
_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  0.0586
_diffrn_reflns_av_unetI/netI     0.0627
_diffrn_reflns_Laue_measured_fraction_full 0.808
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            72196
_diffrn_reflns_point_group_measured_fraction_full 0.705
_diffrn_reflns_point_group_measured_fraction_max 0.873
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         23.397
_diffrn_reflns_theta_min         1.050
_exptl_absorpt_coefficient_mu    1.064
_exptl_absorpt_correction_T_max  0.845
_exptl_absorpt_correction_T_min  0.700
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_description       prism
_exptl_crystal_F_000             3104
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.290
_exptl_crystal_size_min          0.150
_platon_squeeze_details
;
 It was not possible to unambiguously identify the disordered solvent(s).
 Since there are 248 electrons in all which gives 33 electrons per
 asymmetric unit, it is possible that this unit contains 1/2 molecule of
 chloroform or 1/2 molecule of isopropyl ether (in both cases,
 58/2=29 electrons). This gives 232 electrons, not too far away from the number
 of electrons estimated by PLATON SQUEEZE. Thus, the unit cell should
 contain additional 4 chloroform molecules or 4 isopropyl ether molecules.
 The refinements without and with SQUEEZE treatment gave R1 factors of
 10.06% and 4.87%, respectively, and thus the solvent-masking improved
 the result by 51.6%. 
 The doubt in identifying the disordered molecules prevented their
 explicit inclusion into the CIF.
;
_refine_diff_density_max         1.413
_refine_diff_density_min         -0.782
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details
;
 Flack x determined using 5230 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.009(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1407
_refine_ls_number_reflns         18315
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0487
_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^)+(0.0809P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1242
_refine_ls_wR_factor_ref         0.1307
_reflns_Friedel_coverage         0.662
_reflns_Friedel_fraction_full    0.592
_reflns_Friedel_fraction_max     0.735
_reflns_number_gt                15336
_reflns_number_total             18315
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt01917b2.cif
_cod_data_source_block           Compound12
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 7032046--7032050.cif.
;
_cod_database_code               7032048
_shelx_estimated_absorpt_t_min   0.694
_shelx_estimated_absorpt_t_max   0.857
_shelxl_version_number           2013-4
_shelx_res_checksum              80642