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_7226648
_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, 1.56(C H4 O), 0.88(H2 O)'
_chemical_formula_sum            'C41.56 H48 N8 O10.44'
_chemical_formula_weight         826.64
_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
;
2016-07-28 deposited with the CCDC.
2016-09-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 119.075(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.177(10)
_cell_length_b                   7.999(2)
_cell_length_c                   21.586(7)
_cell_measurement_reflns_used    4727
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      28.4967
_cell_measurement_theta_min      1.5970
_cell_volume                     4403(2)
_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    'SIR 2014 (Burla, 2015)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.891
_diffrn_measurement_device_type  'Rigaku AFc7S'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0941
_diffrn_reflns_av_unetI/netI     0.1248
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.891
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            17194
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.700
_diffrn_reflns_theta_min         1.597
_diffrn_source                   'Sealed tube'
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5710
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_description       needle
_exptl_crystal_F_000             1748
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         5080
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.2146
_refine_ls_R_factor_gt           0.1105
_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^)+(0.1408P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2591
_refine_ls_wR_factor_ref         0.3272
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2353
_reflns_number_total             5080
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01800a2.cif
_cod_data_source_block           wat_met
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7226643--7226648.cif.
;
_cod_database_code               7226648
_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
 Sof(O2S)=1-FVAR(1)
 Sof(C1S)=Sof(H1SA)=Sof(H1SB)=Sof(H1SC)=FVAR(1)
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              25812
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'