Supramolecular Double-Helix Formation by Diastereoisomeric Conformations of Configurationally Enantiomeric Macrocycles.
Samanta, Avik; Liu, Zhichang; Nalluri, Siva Krishna Mohan; Zhang, Yu; Schatz, George C.; Stoddart, J. Fraser; Journal of the American Chemical Society 138 (2016) 14469–14480; doi:10.1021/jacs.6b09258

data_4125294
_publ_section_title
;
 Supramolecular Double-Helix Formation by Diastereoisomeric Conformations
 of Configurationally Enantiomeric Macrocycles.
;
_journal_issue                   43
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14469
_journal_page_last               14480
_journal_paper_doi               10.1021/jacs.6b09258
_journal_volume                  138
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C44 H32 N4 O8, C H4 O'
_chemical_formula_sum            'C45 H36 N4 O9'
_chemical_formula_weight         776.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-10-13
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.500(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.045(4)
_cell_length_b                   8.2580(9)
_cell_length_c                   14.0706(15)
_cell_measurement_reflns_used    9877
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.169
_cell_measurement_theta_min      3.935
_cell_volume                     3691.6(7)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 V2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Kappa Apex 2'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_Laue_measured_fraction_full 0.945
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19174
_diffrn_reflns_point_group_measured_fraction_full 0.930
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.179
_diffrn_reflns_theta_min         3.168
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    0.812
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.6580
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1419 before and 0.0470 after correction.
The Ratio of minimum to maximum transmission is 0.8743.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_description       needle
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.446
_exptl_crystal_size_mid          0.286
_exptl_crystal_size_min          0.024
_refine_diff_density_max         0.212
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Flack x determined using 2770 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.01(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         6201
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0642P)^2^+1.9901P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1008
_reflns_Friedel_coverage         0.830
_reflns_Friedel_fraction_full    0.912
_reflns_Friedel_fraction_max     0.962
_reflns_number_gt                6133
_reflns_number_total             6201
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b09258_si_001.cif
_cod_data_source_block           cx0582
_cod_depositor_comments
'Adding full bibliography for 4125292--4125294.cif.'
_cod_database_code               4125294
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.713
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C6(H6), C23(H23), C28(H28)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C24(H24A,H24B), C25(H25A,
 H25B), C26(H26A,H26B), C27(H27A,H27B)
2.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C12(H12), C16(H16), C21(H21), C22(H22), C31(H31), C32(H32),
 C34(H34), C38(H38), C43(H43), C44(H44)
2.d Idealised Me refined as rotating group:
 C45(H45A,H45B,H45C)
2.e Idealised tetrahedral OH refined as rotating group:
 O9(H9A)
;
_shelx_res_checksum              46656
_shelx_hkl_checksum              94986
_olex2_date_sample_data_collection 2015-10-12
_olex2_date_sample_submission    2015-10-09
_olex2_submission_original_sample_id cx0582
_olex2_submission_special_instructions 'No special instructions were received'