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_7226644
_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         'C30 H30 N6 O6, 2(O H2), 2(C2 H6 O S)'
_chemical_formula_sum            'C34 H46 N6 O10 S2'
_chemical_formula_weight         762.89
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-21
_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                 102.255(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.022(2)
_cell_length_b                   17.377(3)
_cell_length_c                   8.6788(15)
_cell_measurement_reflns_used    4993
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      28.3389
_cell_measurement_theta_min      1.6001
_cell_volume                     1919.1(6)
_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    'SIR2014 (Burla et al., 2015)'
_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 0.993
_diffrn_measured_fraction_theta_max 0.971
_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  0.1135
_diffrn_reflns_av_unetI/netI     0.1515
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            15304
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.519
_diffrn_reflns_theta_min         1.600
_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    0.201
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             808
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile/water/DMSO'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.937
_refine_diff_density_min         -1.119
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         4720
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1987
_refine_ls_R_factor_gt           0.1145
_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          0.2724
_refine_ls_wR_factor_ref         0.3630
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2202
_reflns_number_total             4720
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01800a2.cif
_cod_data_source_block           ale26_31_1
_cod_depositor_comments
'Adding full bibliography for 7226643--7226648.cif.'
_cod_database_code               7226644
_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
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C13(H13A,H13B), C7(H7A,H7B), C12(H12A,H12B), C8(H8A,
 H8B)
2.b Idealised Me refined as rotating group:
 C1S(H2S,H3S,H1S), C2S(H5S,H4S,H6S)
2.c :
 C5(H5), C10(H10), C15(H15)
;
_shelx_res_checksum              54555
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_completion    2015-11-10
_olex2_date_sample_data_collection 2015-11-09
_olex2_submission_special_instructions 'No special instructions were received'