Waste reduction in amide synthesis by a continuous method based on recycling of the reaction mixture
Thalluri, Kishore; Nadimpally, Krishna Chaitanya; Paul, Ashim; Mandal, Bhubaneswar; RSC Advances 2 (2012) 6838–; doi:10.1039/c2ra20643a

data_7238667
_publ_section_title
;
 Waste reduction in amide synthesis by a continuous method based on
 recycling of the reaction mixture
;
_journal_issue                   17
_journal_name_full               'RSC Advances'
_journal_page_first              6838
_journal_paper_doi               10.1039/c2ra20643a
_journal_volume                  2
_journal_year                    2012
_chemical_formula_sum            'C14 H19 N O'
_chemical_formula_weight         217.30
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        '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                79.59(3)
_cell_angle_beta                 73.54(4)
_cell_angle_gamma                73.58(3)
_cell_formula_units_Z            4
_cell_length_a                   9.493(5)
_cell_length_b                   11.707(5)
_cell_length_c                   12.816(6)
_cell_measurement_temperature    296(2)
_cell_volume                     1302.4(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_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  0.0702
_diffrn_reflns_av_sigmaI/netI    0.0838
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8043
_diffrn_reflns_theta_full        20.23
_diffrn_reflns_theta_max         20.23
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.069
_exptl_crystal_density_diffrn    1.108
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             472
_refine_diff_density_max         0.169
_refine_diff_density_min         -0.192
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.908
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         2452
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.908
_refine_ls_R_factor_all          0.1314
_refine_ls_R_factor_gt           0.0672
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1619
_refine_ls_wR_factor_ref         0.2003
_reflns_number_gt                1125
_reflns_number_total             2452
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ra20643a.txt
_cod_data_source_block           1
_cod_original_cell_volume        1302.5(11)
_cod_database_code               7238667