Chiroptical sensing of oligonucleotides with a cyclic octapyrrole
Ie, Machiko; Setsune, Jun-ichiro; Eda, Kazuo; Tsuda, Akihiko; Organic Chemistry Frontiers 2 (2015) 29–; doi:10.1039/C4QO00268G

data_1553042
_publ_section_title
;
 Chiroptical sensing of oligonucleotides with a cyclic octapyrrole
;
_journal_issue                   1
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              29
_journal_paper_doi               10.1039/C4QO00268G
_journal_volume                  2
_journal_year                    2015
_chemical_formula_moiety         'C86 H92 N8, C6 H6'
_chemical_formula_sum            'C92 H98 N8'
_chemical_formula_weight         1315.79
_space_group_IT_number           34
_space_group_name_Hall           'P 2 -2n'
_space_group_name_H-M_alt        'P n n 2'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 -2n'
_symmetry_space_group_name_H-M   'P n n 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/cc13hfpq
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-10-08 deposited with the CCDC.
2014-11-28 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.865(4)
_cell_length_b                   16.430(4)
_cell_length_c                   14.961(4)
_cell_measurement_reflns_used    6318
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.62
_cell_measurement_theta_min      2.25
_cell_volume                     3899.8(17)
_computing_cell_refinement       'APEXII (Bruker AXS, 2006)'
_computing_data_collection       'APEXII (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'Bruker XSHELL ver. 6.3.1'
_computing_publication_material  'Bruker XSHELL ver. 6.3.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0305
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18780
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_T_max  0.9747
_exptl_absorpt_correction_T_min  0.9345
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'program SADABS ver. 2.03(Sheldrick)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.120
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1412.0
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_platon_squeeze_details
; 
 This equates to 8 e-/cell, and is interpreted as a real void. Without the 
 disorder structure of the methyl and isobutyl groups, volume of the 
 void increases up to 90 ang3. We suppose that one acetonitrile molecule,  
 used as a recrystallization solvent, was in the void, since one  
 acetonitrile molecule is calculated to occupy ca. 100 ang3. This 
 acetonitrile molecule is easily released from the crystal.
;
_refine_diff_density_max         0.201
_refine_diff_density_min         -0.150
_refine_diff_density_rms         0.033
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         6562
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0433
_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^)+(0.0622P)^2^+0.5462P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1077
_refine_ls_wR_factor_ref         0.1132
_reflns_number_gt                5728
_reflns_number_total             6562
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4qo00268g2.cif
_cod_data_source_block           140930_1_0ma
_cod_original_cell_volume        3899.7(17)
_cod_original_sg_symbol_Hall     'P 2 -2n '
_cod_database_code               1553042