A General Synthetic Route to Isomeric Pyrrolo[1,2- x][1,4]diazepinones.
Zelina, Elena Y.; Nevolina, Tatyana A.; Sorotskaja, Ludmila N.; Skvortsov, Dmitry A.; Trushkov, Igor V.; Uchuskin, Maxim G.; The Journal of organic chemistry 83 (2018) 11747–11757; doi:10.1021/acs.joc.8b01669

data_4035240
_publ_section_title
;
 A General Synthetic Route to Isomeric Pyrrolo[1,2- x][1,4]diazepinones.
;
_journal_issue                   19
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              11747
_journal_page_last               11757
_journal_paper_doi               10.1021/acs.joc.8b01669
_journal_volume                  83
_journal_year                    2018
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C9 H12 N2 O'
_chemical_formula_sum            'C9 H12 N2 O'
_chemical_formula_weight         164.21
_chemical_melting_point          412
_chemical_name_systematic
7-methyl-2,3-dihydro-1H-pyrrolo[1,2-d][1,4]diazepin-4(5H)-one
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2018-05-29T10:30:51-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 103.69(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.958(2)
_cell_length_b                   14.801(5)
_cell_length_c                   8.546(2)
_cell_measurement_reflns_used    1336
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.1400
_cell_measurement_theta_min      4.2250
_cell_measurement_wavelength     0.71073
_cell_volume                     855.1(4)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_pressure         101
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4752
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.9962
_diffrn_measured_fraction_theta_max 0.8551
_diffrn_measurement_details
;
  1 omega  -15.00   98.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       13.8509   19.0000    0.0000 113

  2 omega  -51.00  -16.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.3978  -57.0000   30.0000 35

  3 omega  -16.00   30.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.3978  -99.0000   60.0000 46

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, Ruby'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0261809000
_diffrn_orient_matrix_UB_12      0.0446009000
_diffrn_orient_matrix_UB_13      -0.0168782000
_diffrn_orient_matrix_UB_21      0.0983888000
_diffrn_orient_matrix_UB_22      -0.0144242000
_diffrn_orient_matrix_UB_23      0.0046925000
_diffrn_orient_matrix_UB_31      -0.0252783000
_diffrn_orient_matrix_UB_32      -0.0100663000
_diffrn_orient_matrix_UB_33      -0.0836134000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4077
_diffrn_reflns_theta_full        26.3154
_diffrn_reflns_theta_max         29.3255
_diffrn_reflns_theta_min         3.0132
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             352
_exptl_crystal_recrystallization_method Ethylacetate
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.209
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       0.019(5)
_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   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     116
_refine_ls_number_reflns         2003
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.048
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0607P)^2^+0.1112P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1255
_refine_ls_wR_factor_ref         0.1376
_reflns_number_gt                1586
_reflns_number_total             2003
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            jo8b01669_si_001.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4035240