Cyclic hexapeptoids with N-alkyl side chains: solid-state assembly and thermal behaviour
Pierri, Giovanni; SCHETTINI, ROSARIA; Nuss, Juergen; Dinnebier, Robert E.; De Riccardis, Francesco; Izzo, Irene; Tedesco, Consiglia; CrystEngComm  (2020) –; doi:10.1039/D0CE01136C

data_7241171
_publ_section_title
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 Cyclic hexapeptoids with N-alkyl side chains: solid-state assembly and
 thermal behaviour
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE01136C
_journal_year                    2020
_chemical_formula_moiety         'C42 H78 N6 O6'
_chemical_formula_sum            'C42 H78 N6 O6'
_chemical_formula_weight         763.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-07-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-31 deposited with the CCDC.	2020-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.4256(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3089(17)
_cell_length_b                   15.195(2)
_cell_length_c                   26.307(4)
_cell_measurement_reflns_used    9957
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.45
_cell_measurement_theta_min      2.31
_cell_volume                     4482.7(11)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            35067
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.475
_diffrn_reflns_theta_min         1.551
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  0.2602
_exptl_absorpt_correction_T_min  0.1988
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.0642 before and 0.0495 after correction.
The Ratio of minimum to maximum transmission is 0.7640.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.131
_exptl_crystal_description       plate
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         9226
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0640
_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^)+(0.0835P)^2^+4.5582P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1736
_refine_ls_wR_factor_ref         0.1832
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7534
_reflns_number_total             9226
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01136c2.cif
_cod_data_source_block           form_1LT
_cod_original_cell_volume        4482.5(11)
_cod_database_code               7241171
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C25B, C26B, C27B, C28B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C25B \\sim C26B \\sim C27B \\sim C28B: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
4. Others
 Sof(C6B)=Sof(H6BA)=Sof(H6BB)=Sof(C7B)=Sof(H7BA)=Sof(H7BB)=Sof(H7BC)=1-FVAR(1)
 Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=FVAR(1)
 Sof(H24C)=Sof(H24D)=Sof(C25B)=Sof(H25C)=Sof(H25D)=Sof(C26B)=Sof(H26C)=
 Sof(H26D)=Sof(C27B)=Sof(H27C)=Sof(H27D)=Sof(C28B)=Sof(H28D)=Sof(H28E)=
 Sof(H28F)=1-FVAR(2)
 Sof(H24A)=Sof(H24B)=Sof(C25A)=Sof(H25A)=Sof(H25B)=Sof(C26A)=Sof(H26A)=
 Sof(H26B)=Sof(C27A)=Sof(H27A)=Sof(H27B)=Sof(C28A)=Sof(H28A)=Sof(H28B)=
 Sof(H28C)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6A(H6AA,H6AB), C6B(H6BA,
 H6BB), C8(H8A,H8B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,
 H13B), C15(H15A,H15B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B),
 C20(H20A,H20B), C22(H22A,H22B), C24(H24A,H24B), C24(H24C,H24D), C25A(H25A,
 H25B), C25B(H25C,H25D), C26A(H26A,H26B), C26B(H26C,H26D), C27A(H27A,H27B),
 C27B(H27C,H27D), C29(H29A,H29B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,
 H33B), C34(H34A,H34B), C36(H36A,H36B), C38(H38A,H38B), C39(H39A,H39B),
 C40(H40A,H40B), C41(H41A,H41B)
5.b Idealised Me refined as rotating group:
 C7A(H7AA,H7AB,H7AC), C7B(H7BA,H7BB,H7BC), C14(H14A,H14B,H14C), C21(H21A,H21B,
 H21C), C28A(H28A,H28B,H28C), C28B(H28D,H28E,H28F), C35(H35A,H35B,H35C),
 C42(H42A,H42B,H42C)
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_shelx_res_checksum              98557
_olex2_submission_special_instructions 'No special instructions were received'