Ring size effect on the solid state assembly of propargyl substituted hexa- and octacyclic peptoids
Tedesco, Consiglia; Meli, Alessandra; Macedi, Eleonora; Iuliano, Veronica; Ricciardulli, Antonio G.; De Riccardis, Francesco; Vaughan, Gavin B. M.; Smith, Vincent J.; Barbour, Leonard J.; Izzo, Irene; CrystEngComm 18 (2016) 8838–; doi:10.1039/C6CE01800A

data_7226646
_publ_section_title
;
 Ring size effect on the solid state assembly of propargyl substituted
 hexa- and octacyclic peptoids
;
_journal_issue                   46
_journal_name_full               CrystEngComm
_journal_page_first              8838
_journal_paper_doi               10.1039/C6CE01800A
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C40 H40 N8 O8, (C H4 O),2 (H2 O)'
_chemical_formula_sum            'C41 H48 N8 O11'
_chemical_formula_weight         828.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-06-06
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-07-09 deposited with the CCDC.
2016-09-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 119.615(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.227(11)
_cell_length_b                   7.997(3)
_cell_length_c                   21.680(8)
_cell_measurement_reflns_used    16615
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      28.598
_cell_measurement_theta_min      1.603
_cell_volume                     4405(3)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 13.6612
_diffrn_detector_type            'Rigaku Mercury2'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device       AFC7S
_diffrn_measurement_device_type  Rigaku_AFC7_Mo
_diffrn_measurement_method       dtprofit.ref
_diffrn_measurement_specimen_support 'Mitegen 150um'
_diffrn_radiation_collimation    0.5
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_av_unetI/netI     0.0741
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            16615
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.598
_diffrn_reflns_theta_min         1.603
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_target            Mo
_diffrn_source_type              'Sealed Tube'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_description       needle
_exptl_crystal_F_000             1752
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.660
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         5330
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1474
_refine_ls_R_factor_gt           0.0967
_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^)+(0.1007P)^2^+6.7458P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2380
_refine_ls_wR_factor_ref         0.2725
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3060
_reflns_number_total             5330
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01800a2.cif
_cod_data_source_block           ale60_b2_1bis
_cod_depositor_comments
'Adding full bibliography for 7226643--7226648.cif.'
_cod_database_code               7226646
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Others
 Fixed Sof: C1S(0.5) H1SA(0.5) H1SB(0.5) H1SC(0.5) O2S(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C7(H7A,H7B), C8(H8A,H8B), C12(H12A,H12B), C13(H13A,
 H13B), C17(H17A,H17B), C18(H18A,H18B)
3.b Idealised Me refined as rotating group:
 C1S(H1SA,H1SB,H1SC)
3.c Idealised tetrahedral OH refined as rotating group:
 O1S(H1S)
3.d :
 C5(H5), C10(H10), C15(H15), C20(H20)
;
_shelx_res_checksum              12019
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'