Synthesis and properties of 5,6-dihydrodipyrrolo[1,2-d;2′,1′-g][1,4]diazepin-11-one
Johnston, Karen A.; McNab, Hamish; New Journal of Chemistry 33 (2009) 1703–; doi:10.1039/b906802n

data_7053819
_publ_section_title
;
 Synthesis and properties of
 5,6-dihydrodipyrrolo[1,2-d;2&#x2032;,1&#x2032;-g][1,4]diazepin-11-one
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1703
_journal_paper_doi               10.1039/b906802n
_journal_volume                  33
_journal_year                    2009
_chemical_compound_source        'Karen Johnston'
_chemical_formula_moiety         'C10 H8 N2 O'
_chemical_formula_sum            'C10 H8 N2 O'
_chemical_formula_weight         172.18
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   '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                102.228(2)
_cell_angle_beta                 93.332(2)
_cell_angle_gamma                99.815(2)
_cell_formula_units_Z            4
_cell_length_a                   7.6509(2)
_cell_length_b                   9.1569(3)
_cell_length_c                   12.0975(4)
_cell_measurement_temperature    150(2)
_cell_volume                     812.26(4)
_computing_molecular_graphics    Shelxp
_computing_publication_material  'Platon, encifer'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Shelxs Sheldrick'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       'Omega Scans'
_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  0.0416
_diffrn_reflns_av_sigmaI/netI    0.0579
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11866
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         30.53
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  0.9849
_exptl_absorpt_correction_T_min  0.8167
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             360
_exptl_crystal_recrystallization_method
'Evaporation of Chloroform/Toluene Solution'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         4583
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_gt           0.0597
_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^)+(0.0520P)^2^+0.2206P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1247
_refine_ls_wR_factor_ref         0.1396
_reflns_number_gt                3122
_reflns_number_total             4583
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b906802nsup1.cif
_cod_data_source_block           hm7004
_cod_database_code               7053819