One-pot synthesis of γ-lactams in a reaction cascade from α,β-unsaturated imines, CO and ethylene catalysed by Ru3(CO)12†
Berger, Daniel; Imhof, Wolfgang; Chemical Communications  (1999) 1457–; doi:10.1039/a903266e

data_7110575
_publ_section_title
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 One-pot synthesis of \g-lactams in a reaction cascade from
 \a,\b-unsaturated imines, CO and ethylene catalysed by Ru3(CO)12&#x2020;
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_journal_issue                   16
_journal_name_full               'Chemical Communications'
_journal_page_first              1457
_journal_paper_doi               10.1039/a903266e
_journal_year                    1999
_chemical_formula_sum            'C13 H21 N O'
_chemical_formula_weight         207.31
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   20.4759(12)
_cell_length_b                   22.0944(12)
_cell_length_c                   11.4430(4)
_cell_measurement_temperature    293(2)
_cell_volume                     5176.8(5)
_computing_cell_refinement       DENZO
_computing_data_collection       DENZO
_computing_data_reduction        DENZO
_computing_molecular_graphics    XPMA
_computing_publication_material  XP
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measurement_device       KAPPA-CCD
_diffrn_measurement_method       'phi-scan, omega-scan'
_diffrn_radiation_monochromator  graphite
_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    0.0299
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1376
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         3.44
_exptl_absorpt_coefficient_mu    0.066
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.064
_exptl_crystal_description       quader
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.129
_refine_diff_density_min         -0.127
_refine_diff_density_rms         0.026
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -2.05(355)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.081
_refine_ls_goodness_of_fit_obs   1.102
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         1371
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.159
_refine_ls_restrained_S_obs      1.102
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_obs          0.0562
_refine_ls_shift/esd_max         -0.005
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0747P)^2^+4.0404P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1547
_refine_ls_wR_factor_obs         0.1395
_reflns_number_observed          1253
_reflns_number_total             1376
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            903266esup1.cif
_cod_data_source_block           tt1024
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0747P)^2^+4.0404P] 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^)+(0.0747P)^2^+4.0404P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      Fdd2
_cod_database_code               7110575