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_7241174
_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         'C24 H19 N3 O3'
_chemical_formula_sum            'C24 H19 N3 O3'
_chemical_formula_weight         397.42
_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
_audit_creation_date             2020-07-31
_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.
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_cell_angle_alpha                90
_cell_angle_beta                 103.204(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.888(15)
_cell_length_b                   15.377(14)
_cell_length_c                   11.247(10)
_cell_measurement_reflns_used    1923
_cell_measurement_temperature    360(2)
_cell_measurement_theta_max      25.15
_cell_measurement_theta_min      2.39
_cell_volume                     2843(4)
_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      360.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0961
_diffrn_reflns_av_unetI/netI     0.0915
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            18451
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.478
_diffrn_reflns_theta_min         1.239
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1596 before and 0.0670 after correction.
The Ratio of minimum to maximum transmission is 0.7936.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.928
_exptl_crystal_description       plate
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.702
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.308
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.281
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         5208
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.280
_refine_ls_R_factor_all          0.2911
_refine_ls_R_factor_gt           0.1524
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3827
_refine_ls_wR_factor_ref         0.4591
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1946
_reflns_number_total             5208
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01136c2.cif
_cod_data_source_block           55_now
_cod_database_code               7241174
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C19A-C20B = C23B-C22B
 1.5418 with sigma of 0.01
 C14B-C15 = C15-C16
 1.5418 with sigma of 0.01
 C23A-C24B
 1.5418 with sigma of 0.01
 C23B-C23A
 1.5418 with sigma of 0.02
 C22B-C23B
 1.5418 with sigma of 0.02
 C23B-C24B
 1.5418 with sigma of 0.02
 C24A-C23A
 1.5418 with sigma of 0.02
3. Others
 Fixed Sof: C13A(0.5) C23A(0.5) C14B(0.5) C19A(0.5) C19B(0.5) C20B(0.5)
 C21B(0.5) C23B(0.5) C22B(0.5) C20A(0.5) C21A(0.5) C22A(0.5) C24B(0.5) C3AA(0.5)
4.a Free rotating group:
 C11(C12A)
4.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B),
 C9(H9A,H9B), C17(H17A,H17B)
4.c Me refined with riding coordinates:
 C8(H8A,H8B,H8C)
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_shelx_res_checksum              55233
_olex2_submission_special_instructions 'No special instructions were received'