Solvent-free microwave-assisted Meyers’ lactamization
Jida, Mouhamad; Deprez-Poulain, Rebecca; Malaquin, Sandra; Roussel, Pascal; Agbossou-Niedercorn, Francine; Deprez, Benoit; Laconde, Guillaume; Green Chemistry 12 (2010) 961–; doi:10.1039/b924111f

data_7212282
_publ_section_title
;
 Solvent-free microwave-assisted Meyers&#x2019; lactamization
;
_journal_issue                   6
_journal_name_full               'Green Chemistry'
_journal_page_first              961
_journal_paper_doi               10.1039/b924111f
_journal_volume                  12
_journal_year                    2010
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C12 H17 N1 O4'
_chemical_formula_sum            'C12 H17 N O4'
_chemical_formula_weight         239.27
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 113.780(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5352(8)
_cell_length_b                   7.6758(4)
_cell_length_c                   10.0025(4)
_cell_measurement_reflns_used    5996
_cell_measurement_temperature    293
_cell_measurement_theta_max      24
_cell_measurement_theta_min      2
_cell_volume                     1232.00(10)
_computing_cell_refinement       'SAINT (Siemens ,1995)'
_computing_data_collection       'SMART (Siemens, 1993)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       'Bruker SMART'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.045
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23846
_diffrn_reflns_theta_full        35.708
_diffrn_reflns_theta_max         36.437
_diffrn_reflns_theta_min         2.225
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            transparent
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.17
_refine_diff_density_min         -0.23
_refine_ls_extinction_coef       50(11)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0751
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2041
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1102
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.000078
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
2.21 -0.251 1.59 -0.249 0.269
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0747
_refine_ls_wR_factor_gt          0.0458
_refine_ls_wR_factor_ref         0.0431
_reflns_limit_h_max              26
_reflns_limit_h_min              -29
_reflns_limit_k_max              12
_reflns_limit_k_min              -12
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                2376
_reflns_number_total             5724
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0407
_oxford_refine_ls_scale          2.266(5)
_oxford_reflns_number_all        5714
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            b924111f.txt
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 
;
_cod_original_sg_symbol_H-M      'C 1 2 1 '
_cod_original_formula_sum        'C12 H17 N1 O4'
_cod_database_code               7212282