Structural adaptations of electrosprayed aromatic oligoamide foldamers on Ag(111)
Meier, Dennis; Schoof, Benedikt; Wang, Jinhua; Li, Xuesong; Walz, Andreas; Huettig, Annette; Schlichting, Hartmut; Rosu, Frédéric; Gabelica, Valérie; Maurizot, Victor; Reichert, Joachim; Papageorgiou, Anthoula C.; Huc, Ivan; Barth, Johannes V.; Chemical Communications  (2022) –; doi:10.1039/D2CC03286D

data_7130347
_publ_section_title
;
 Structural adaptations of electrosprayed aromatic oligoamide foldamers on
 Ag(111)
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC03286D
_journal_year                    2022
_chemical_formula_moiety         'C74 H68 N8 O10'
_chemical_formula_sum            'C74 H68 N8 O10'
_chemical_formula_weight         1229.36
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.12.01 svn.r5f60950 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-01-21 deposited with the CCDC.	2022-07-10 downloaded from the CCDC.
;
_cell_angle_alpha                110.870(2)
_cell_angle_beta                 91.168(2)
_cell_angle_gamma                99.895(2)
_cell_formula_units_Z            2
_cell_length_a                   12.1814(2)
_cell_length_b                   16.7246(3)
_cell_length_c                   17.9169(3)
_cell_measurement_reflns_used    32619
_cell_measurement_temperature    130
_cell_measurement_theta_max      73.6320
_cell_measurement_theta_min      2.8670
_cell_volume                     3346.74(11)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      130
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Rigaku FRX'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0151
_diffrn_reflns_av_unetI/netI     0.0125
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            39409
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.067
_diffrn_reflns_theta_min         2.881
_exptl_absorpt_coefficient_mu    0.665
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.54720
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.120a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_description       block
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.103
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       0.0042(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     850
_refine_ls_number_reflns         12525
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0560
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+1.4903P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1585
_refine_ls_wR_factor_ref         0.1601
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11827
_reflns_number_total             12525
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03286d2.cif
_cod_data_source_block           wj_pyq4_ref_b
_cod_database_code               7130347
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 C01X, O009
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C2, C01X
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=1-FVAR(1)
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C01Q(H01Q), C01T(H01T), C02G(H02S), C2(H2)
4.b Secondary CH2 refined with riding coordinates:
 C01E(H01B,H01C), C01K(H01D,H01E), C01X(H01M,H01N), C024(H02G,H02H)
4.c Aromatic/amide H refined with riding coordinates:
 N00C(H00C), N00E(H00E), N00G(H00G), N00I(H00I), C00K(H00K), C00R(H00R),
 C00V(H00V), C00W(H00W), C012(H012), C017(H017), C018(H018), C019(H019),
 C01A(H01A), C01G(H01G), C01H(H01H), C01I(H01I), C01L(H01L), C01R(H01R),
 C01S(H01S), C01Z(H01Z), C020(H020), C026(H026), C027(H027), C028(H028),
 C029(H029), C02A(H02L), C02C(H02M), C02D(H02N), C02F(H02R)
4.d Idealised Me refined as rotating group:
 C01W(H01F,H01J,H01K), C021(H02A,H02B,H02C), C023(H02D,H02E,H02F), C025(H02I,
 H02J,H02K), C02E(H02O,H02P,H02Q), C02J(H02T,H02U,H02V), C02O(H02W,H02X,H02Y),
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C3A(H3AA,H3AB,H3AC)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              63684
_shelx_hkl_checksum              24665
_shelx_fab_checksum              73491
_olex2_submission_original_sample_id wj_Q4pyr
_olex2_submission_special_instructions 'No special instructions were received'