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_7212281
_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_sum            'C18 H20 N2 O2'
_chemical_formula_weight         296.40
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 98.698(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.4078(8)
_cell_length_b                   8.3744(8)
_cell_length_c                   11.4399(10)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    293
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     796.22(13)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_data_reduction        'USER DEFINED DATA REDUCTION'
_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    'USER DEFINED STRUCTURE SOLUTION'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       Unknown
_diffrn_measurement_device_type  Serial
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            47945
_diffrn_reflns_theta_full        26.463
_diffrn_reflns_theta_max         26.463
_diffrn_reflns_theta_min         1.801
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  1.0000
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             316
_refine_diff_density_max         0.12
_refine_diff_density_min         -0.12
_refine_ls_extinction_coef       30(12)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.1559
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         1411
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.004502
_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:
0.470 0.403 0.210 0.338E-01 0.206E-01
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0746
_refine_ls_wR_factor_gt          0.0441
_refine_ls_wR_factor_ref         0.0431
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                1463
_reflns_number_total             1767
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   4.60
_oxford_diffrn_Wilson_scale      1.51
_oxford_refine_ls_r_factor_ref   0.0381
_oxford_refine_ls_scale          1.131(3)
_oxford_reflns_number_all        1757
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            b924111f.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21 '
_cod_original_formula_sum        'C2.25 H2.50 N0.25 O0.25'
_cod_database_code               7212281