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_2104301
_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         'C44 H32 O6 N4, C2 H6 O S, H2 O'
_chemical_formula_sum            'C46 H40 N4 O8 S'
_chemical_formula_weight         808.88
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.14(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.374(4)
_cell_length_b                   9.319(2)
_cell_length_c                   20.515(4)
_cell_measurement_reflns_used    2240
_cell_measurement_temperature    130.0(5)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      4.00
_cell_volume                     4015.9(16)
_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      130.0(5)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0529
_diffrn_reflns_av_sigmaI/netI    0.0581
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13581
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         4.00
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 'every 50 dc frames'
_exptl_absorpt_coefficient_mu    0.142
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.882
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SCALE3 ABSPACK.Oxford Diffraction program,2002.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1693.1
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.206
_refine_diff_density_min         -0.195
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.05(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         3769
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0343P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0718
_refine_ls_wR_factor_ref         0.0775
_reflns_number_gt                3166
_reflns_number_total             3769
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            so5018.cif
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               2104301
_cod_database_fobs_code          2104301