Structurally diverse arene-fused ten-membered lactams accessed via hydrolytic imidazoline ring expansion.
Sapegin, Alexander; Osipyan, Angelina; Krasavin, Mikhail; Organic & biomolecular chemistry 15 (2017) 2906–2909; doi:10.1039/c7ob00535k

data_7155535
_publ_section_title
;
 Structurally diverse arene-fused ten-membered lactams accessed via
 hydrolytic imidazoline ring expansion.
;
_journal_issue                   14
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              2906
_journal_page_last               2909
_journal_paper_doi               10.1039/c7ob00535k
_journal_volume                  15
_journal_year                    2017
_chemical_formula_moiety         'C15 H13 N4 O4'
_chemical_formula_sum            'C15 H14 N4 O4'
_chemical_formula_weight         314.30
_chemical_name_systematic
'8-Methyl-2-nitro-7,8-dihydro-5H-benzo[i]pyrido[3,2-b][1,4,7]oxadiazecin-9(6H)-one '
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-12-05
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2016-12-05 deposited with the CCDC.
2017-03-14 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.0497(7)
_cell_length_b                   11.1392(5)
_cell_length_c                   16.514(5)
_cell_measurement_temperature    293(2)
_cell_volume                     2768.4(9)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11083
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.59
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.099
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1148
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: propanol-2'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.874
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3167
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+1.6886P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0967
_refine_ls_wR_factor_ref         0.1032
_reflns_number_gt                2614
_reflns_number_total             3167
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7ob00535k2.cif
_cod_data_source_block           mk-1
_cod_depositor_comments
;
          Adding full bibliography for 7155535.cif.

2018-03-13
Z value changed to be consistent with given formula                 miguel
;
_cod_original_formula_moiety         '1.14(C15 H13 N4 O4)'
_cod_original_formula_units_Z            7
_cod_original_cell_volume        2768.5(8)
_cod_database_code               7155535
_olex2_refinement_description
;
;
_olex2_submission_special_instructions 'No special instructions were received'