Probing the shapes of chiral bis-(<i>o</i>-naphthalimidobenzoyl) systems using X-ray and circular dichroism methods
Rychlewska, Urszula; Plutecka, Agnieszka; Hoffmann, Marcin; Skowronek, Paweł; Gawrońska, Krystyna; Gawroński, Jacek; Acta Crystallographica Section B 65 (2009) 86–95; doi:10.1107/S0108768108041827

data_2104299
_publ_section_title
;
 Probing the shapes of chiral bis-(<i>o</i>-naphthalimidobenzoyl)
 systems using X-ray and circular dichroism methods
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              86
_journal_page_last               95
_journal_paper_doi               10.1107/S0108768108041827
_journal_volume                  65
_journal_year                    2009
_chemical_formula_moiety         'C43 H30 N2 O8'
_chemical_formula_sum            'C43 H30 N2 O8'
_chemical_formula_weight         702.69
_space_group_IT_number           1
_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                103.203(6)
_cell_angle_beta                 111.486(7)
_cell_angle_gamma                107.147(6)
_cell_formula_units_Z            1
_cell_length_a                   9.2897(7)
_cell_length_b                   10.0849(7)
_cell_length_c                   11.0897(8)
_cell_measurement_reflns_used    4689
_cell_measurement_temperature    140.0(5)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      3.17
_cell_volume                     855.11(14)
_computing_cell_refinement
'CrysAlisRED v.1.171.23(Oxford Diffraction,2002)'
_computing_data_collection
'CrysAlisCCD v.1.171.23(Oxford Diffraction,2002)'
_computing_data_reduction
'CrysAlisRED v.1.171.23(Oxford Diffraction,2002)'
_computing_molecular_graphics
'XP. Simens Analytical X-Ray Instruments (1989)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Kuma KM4CCD \k-geometry diffractometer'
_diffrn_measurement_method       '\w 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  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8911
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.17
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 'every 50 dc frames'
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             366
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.156
_refine_diff_density_min         -0.179
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(10)
_refine_ls_extinction_coef       0.038(3)
_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   0.911
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         2994
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.911
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0311
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0549
_refine_ls_wR_factor_ref         0.0577
_reflns_number_gt                2388
_reflns_number_total             2994
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            so5018.cif
_cod_data_source_block           2
_cod_database_code               2104299
_cod_database_fobs_code          2104299