Synthesis and characterization of new Na+ complexes of N-benzyl cyclic peptoids and their role in the ring opening polymerization of l-lactide
D'Amato, Assunta; Schettini, Rosaria; Pierri, Giovanni; Izzo, Irene; Grisi, Fabia; Tedesco, Consiglia; De Riccardis, Francesco; Costabile, Chiara; New Journal of Chemistry 45 (2021) 5410–5420; doi:10.1039/D0NJ05931E

data_7060437
_publ_section_title
;
 Synthesis and characterization of new Na+ complexes of N-benzyl cyclic
 peptoids and their role in the ring opening polymerization of l-lactide
;
_journal_issue                   12
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              5410
_journal_page_last               5420
_journal_paper_doi               10.1039/D0NJ05931E
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C118 H78 B2 F48 N6 Na2 O8, 2(C H Cl3)'
_chemical_formula_sum            'C120 H80 B2 Cl6 F48 N6 Na2 O8'
_chemical_formula_weight         2926.20
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-01-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-28 deposited with the CCDC.	2021-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                97.25(2)
_cell_angle_beta                 105.386(19)
_cell_angle_gamma                105.82(3)
_cell_formula_units_Z            1
_cell_length_a                   13.193(9)
_cell_length_b                   14.898(10)
_cell_length_c                   18.494(10)
_cell_measurement_reflns_used    9828
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      71.06
_cell_measurement_theta_min      3.15
_cell_volume                     3294(4)
_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 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.947
_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  0.0683
_diffrn_reflns_av_unetI/netI     0.0597
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            51944
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.479
_diffrn_reflns_theta_min         2.537
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.369
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.4818
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1361 before and 0.0776 after correction.
The Ratio of minimum to maximum transmission is 0.6393.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_description       prism
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       0.0078(11)
_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   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1114
_refine_ls_number_reflns         12383
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1339
_refine_ls_R_factor_gt           0.1007
_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^)+(0.1728P)^2^+2.5710P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2795
_refine_ls_wR_factor_ref         0.3116
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8298
_reflns_number_total             12383
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj05931e2.cif
_cod_data_source_block           reb721_natfpb_0m_a_ok
_cod_depositor_comments          'Adding full bibliography for 7060437.cif.'
_cod_database_code               7060437
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 F22B-F23B \\sim F22B-F24B \\sim F23B-F24B \\sim F22A-F23A \\sim F22A-F24A
\\sim F23A-F24A
 with sigma of 0.04
 C59-F22B \\sim C59-F23B \\sim C59-F24B \\sim C59-F22A \\sim C59-F23A \\sim
C59-F24A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1SA \\sim Cl1A \\sim Cl2A \\sim Cl3A: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C1SB \\sim Cl1B \\sim Cl2B \\sim Cl3B: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 C1SA, Cl1A, Cl2A, Cl3A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1SB, Cl1B, Cl2B, Cl3B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F16B)=Sof(F17B)=Sof(F18B)=1-FVAR(1)
 Sof(F16A)=Sof(F17A)=Sof(F18A)=FVAR(1)
 Sof(F13B)=Sof(F14B)=Sof(F15B)=1-FVAR(2)
 Sof(F13A)=Sof(F14A)=Sof(F15A)=FVAR(2)
 Sof(F19B)=Sof(F20B)=Sof(F21B)=1-FVAR(3)
 Sof(F19A)=Sof(F20A)=Sof(F21A)=FVAR(3)
 Sof(F7B)=Sof(F8B)=Sof(F9B)=1-FVAR(4)
 Sof(F7A)=Sof(F8A)=Sof(F9A)=FVAR(4)
 Sof(F10B)=Sof(F11B)=Sof(F12B)=1-FVAR(5)
 Sof(F10A)=Sof(F11A)=Sof(F12A)=FVAR(5)
 Sof(F22B)=Sof(F23B)=Sof(F24B)=1-FVAR(6)
 Sof(F22A)=Sof(F23A)=Sof(F24A)=FVAR(6)
 Sof(F4B)=Sof(F5B)=Sof(F6B)=1-FVAR(7)
 Sof(F4A)=Sof(F5A)=Sof(F6A)=FVAR(7)
 Sof(F1B)=Sof(F2B)=Sof(F3B)=1-FVAR(8)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=FVAR(8)
 Fixed Sof: C1SA(0.5) H1SA(0.5) Cl1A(0.5) Cl2A(0.5) Cl3A(0.5) C1SB(0.5)
 H1SB(0.5) Cl1B(0.5) Cl2B(0.5) Cl3B(0.5)
6.a Free rotating group:
 C1SA(Cl1A,Cl2A,Cl3A), C1SB(Cl1B,Cl2B,Cl3B)
6.b Ternary CH refined with riding coordinates:
 C1SA(H1SA), C1SB(H1SB)
6.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C10(H10A,H10B), C12(H12A,H12B), C19(H19A,H19B),
 C21(H21A,H21B)
6.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C29(H29),
  C31(H31), C33(H33), C37(H37), C39(H39), C41(H41), C45(H45), C47(H47),
 C49(H49), C53(H53), C55(H55), C57(H57)
;
_shelx_res_checksum              95273
_olex2_submission_special_instructions 'No special instructions were received'