Rhodium(III)-mediated oxime‒nitrile coupling giving chelated iminoacylated species †
Yu. Kukushkin, Vadim; Ilichev, Igor V.; Wagner, Gabriele; Fraústo da Silva, João J. R.; Pombeiro, Armando J. L.; Journal of the Chemical Society, Dalton Transactions  (1999) 3047–; doi:10.1039/a903844b

data_7027546
_publ_section_title
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 Rhodium(III)-mediated oxime--nitrile coupling giving chelated
 iminoacylated species&#x200A;&#x2020;
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_journal_issue                   17
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3047
_journal_paper_doi               10.1039/a903844b
_journal_year                    1999
_chemical_formula_sum            'C14 H27 Cl3 N4 O3.5 Rh'
_chemical_formula_weight         516.66
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                67.21(3)
_cell_angle_beta                 94.35(3)
_cell_angle_gamma                82.12(3)
_cell_formula_units_Z            2
_cell_length_a                   8.524(2)
_cell_length_b                   11.529(2)
_cell_length_c                   12.116(2)
_cell_measurement_reflns_used    15
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     1076.5(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.815
_diffrn_measured_fraction_theta_max 0.815
_diffrn_measurement_device_type  'Syntex P-1'
_diffrn_measurement_method       theta/2theta
_diffrn_radiation_monochromator  beta-filter
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0147
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3103
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        2
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.188
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             526
_exptl_crystal_size_max          .52
_exptl_crystal_size_mid          .50
_exptl_crystal_size_min          .10
_refine_diff_density_max         0.969
_refine_diff_density_min         -1.325
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       0.0108(16)
_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   1.045
_refine_ls_hydrogen_treatment    refined
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     343
_refine_ls_number_reflns         3103
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.750
_refine_ls_shift/su_mean         0.073
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0608P)^2^+0.9751P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0828
_reflns_number_gt                3094
_reflns_number_total             3103
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            903844bsup1.cif
_cod_data_source_block           pmb21
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0608P)^2^+0.9751P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0608P)^2^+0.9751P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1076.5(4)
_cod_original_formula_sum        'C14 H27 Cl3 N4 O3.50 Rh'
_cod_database_code               7027546