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_7241175
_publ_section_title
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 Cyclic hexapeptoids with N-alkyl side chains: solid-state assembly and
 thermal behaviour
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_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             2019-10-10
_audit_creation_method
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
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_audit_update_record
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2020-07-28 deposited with the CCDC.	2020-09-02 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 108.980(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.6731(11)
_cell_length_b                   15.3415(10)
_cell_length_c                   11.2315(8)
_cell_measurement_reflns_used    9953
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      71.59
_cell_measurement_theta_min      4.30
_cell_volume                     2390.8(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            33721
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.287
_diffrn_reflns_theta_min         4.296
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.560
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.6581
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1620 before and 0.0653 after correction.
The Ratio of minimum to maximum transmission is 0.8733.
The \l/2 correction factor is Not present.
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_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.060
_exptl_crystal_description       plate
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.277
_refine_diff_density_min         -0.186
_refine_diff_density_rms         0.035
_refine_ls_extinction_coef       0.023(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   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         4625
_refine_ls_number_restraints     154
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0612
_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^)+(0.1267P)^2^+0.2124P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1815
_refine_ls_wR_factor_ref         0.2031
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3352
_reflns_number_total             4625
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01136c2.cif
_cod_data_source_block           form_1RT
_cod_database_code               7241175
_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
 C12B, C12A, C13B, C13A, C14B, C14A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C4A, C4B, C5A, C6A, C5B, C7A, C6B, C7B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C12A \\sim C13A \\sim C14A \\sim C13B \\sim C12B \\sim C14B: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C4B \\sim C4A \\sim C5A \\sim C5B \\sim C6A \\sim C6B \\sim C7A \\sim C7B:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Others
 Sof(H3BC)=Sof(H3BD)=Sof(C4B)=Sof(H4BA)=Sof(H4BB)=Sof(C5B)=Sof(H5BA)=Sof(H5BB)=
 Sof(C6B)=Sof(H6BA)=Sof(H6BB)=Sof(C7B)=Sof(H7BA)=Sof(H7BB)=Sof(H7BC)=1-FVAR(1)
 Sof(H3AA)=Sof(H3AB)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=
 Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=FVAR(1)
 Sof(H11C)=Sof(H11D)=Sof(C12B)=Sof(H12C)=Sof(H12D)=Sof(C13B)=Sof(H13C)=
 Sof(H13D)=Sof(C14B)=Sof(H14D)=Sof(H14E)=Sof(H14F)=1-FVAR(2)
 Sof(H11A)=Sof(H11B)=Sof(C12A)=Sof(H12A)=Sof(H12B)=Sof(C13A)=Sof(H13A)=
 Sof(H13B)=Sof(C14A)=Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3AA,H3AB), C3(H3BC,H3BD), C4B(H4BA,H4BB), C5B(H5BA,H5BB),
 C6B(H6BA,H6BB), C8(H8A,H8B), C10(H10A,H10B), C11(H11A,H11B), C11(H11C,H11D),
 C12A(H12A,H12B), C13A(H13A,H13B), C15(H15A,H15B), C17(H17A,H17B), C18(H18A,
 H18B), C19(H19A,H19B), C20(H20A,H20B), C5A(H5AA,H5AB), C4A(H4AA,H4AB),
 C6A(H6AA,H6AB), C12B(H12C,H12D), C13B(H13C,H13D)
5.b Me refined with riding coordinates:
 C14A(H14A,H14B,H14C), C7A(H7AA,H7AB,H7AC), C7B(H7BA,H7BB,H7BC), C14B(H14D,
 H14E,H14F)
5.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C)
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_shelx_res_checksum              28987
_olex2_submission_special_instructions 'No special instructions were received'