Foldamer-based helicate displaying reversible switching between two distinct conformers.
Jeon, Hae-Geun; Lee, Hyun Kyung; Lee, Seungwon; Jeong, Kyu-Sung; Chemical communications (Cambridge, England) 54 (2018) 5740–5743; doi:10.1039/c8cc02758g

data_7121704
_publ_section_title
;
 Foldamer-based helicate displaying reversible switching between two
 distinct conformers.
;
_journal_issue                   45
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5740
_journal_page_last               5743
_journal_paper_doi               10.1039/c8cc02758g
_journal_volume                  54
_journal_year                    2018
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C74 H68 N6 O, 2(H2 O)'
_chemical_formula_sum            'C74 H72 N6 O3'
_chemical_formula_weight         1093.37
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-07-17
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-04-05 deposited with the CCDC.
2018-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   35.034(7)
_cell_length_b                   10.393(2)
_cell_length_c                   17.979(4)
_cell_measurement_reflns_used    82091
_cell_measurement_temperature    100
_cell_measurement_theta_max      50
_cell_measurement_theta_min      0.63
_cell_volume                     6546(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13561
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_min         1.599
_diffrn_source                   'Fixed gap multiple wiggler beamline'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.998
_exptl_absorpt_correction_type   Multi-scans
_exptl_absorpt_process_details   HKL3000
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.315
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.846
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Flack x determined using 2933 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   1.0(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     770
_refine_ls_number_reflns         13561
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.1161
_refine_ls_R_factor_gt           0.0818
_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^)+(0.1779P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2256
_refine_ls_wR_factor_ref         0.2451
_reflns_Friedel_coverage         0.809
_reflns_Friedel_fraction_full    0.961
_reflns_Friedel_fraction_max     0.952
_reflns_number_gt                8173
_reflns_number_total             13561
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc02758g2.cif
_cod_data_source_block           IP_tetramer
_cod_depositor_comments
'Adding full bibliography for 7121704--7121706.cif.'
_cod_database_code               7121704
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C68) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C67) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3.a Free rotating group:
 O81(H81D,H81E), O82(H82A,H82B)
3.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N6(H6), N23(H23), N26(H26), C9(H9), C11(H11), C14(H14), C15(H15),
 C18(H18), C20(H20), C29(H29), C31(H31), C34(H34), C35(H35), C38(H38), C40(H40),
  C44(H44), C45(H45), C46(H46), C48(H48), C50(H50), C52(H52)
3.c Idealised Me refined as rotating group:
 C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C67(H67A,H67B,
 H67C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C71(H71A,H71B,H71C), C72(H72A,
 H72B,H72C), C73(H73A,H73B,H73C), C75(H75A,H75B,H75C), C76(H76A,H76B,H76C),
 C77(H77A,H77B,H77C), C79(H79A,H79B,H79C), C80(H80A,H80B,H80C), C81(H81A,H81B,
 H81C)
3.d Idealised tetrahedral OH refined as rotating group:
 O62(H62)
;
_shelx_res_checksum              25322
_shelx_fab_checksum              91604
_olex2_submission_special_instructions 'No special instructions were received'