Impact of flexible succinate connectors on the formation of tetrasulfonylcalix[4]arene based nano-sized polynuclear cages: structural diversity and induced chirality study
Kniazeva, Mariia V.; Ovsyannikov, Alexander S.; Samigullina, Aida I.; Islamov, Daut R.; Gubaidullin, Aidar T.; Dorovatovskii, Pavel V.; Lazarenko, Vladimir A.; Solovieva, Svetlana E.; Antipin, Igor S.; Ferlay, Sylvie; CrystEngComm 24 (2022) 628–638; doi:10.1039/D1CE01482J

data_7244097
_publ_section_title
;
 Impact of flexible succinate connectors on the formation of
 tetrasulfonylcalix[4]arene based nano-sized polynuclear cages: structural
 diversity and induced chirality study
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              628
_journal_page_last               638
_journal_paper_doi               10.1039/D1CE01482J
_journal_volume                  24
_journal_year                    2022
_chemical_absolute_configuration unk
_chemical_formula_moiety
'C96 H104 Ni8 O42 S8, C12 H30 N4 Ni O6, 0.5(H8 O4), 0.5[NC3OH7]'
_chemical_formula_sum            'C108 H138 N4 Ni9 O50 S8'
_chemical_formula_weight         3077.09
_space_group_crystal_system      tetragonal
_space_group_IT_number           94
_space_group_name_Hall           'P 4n 2n'
_space_group_name_H-M_alt        'P 42 21 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_block_doi                 10.5517/ccdc.csd.cc2911r5
_audit_creation_date             2020-01-21
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2021-10-17 deposited with the CCDC.	2021-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   22.981(3)
_cell_length_b                   22.981(3)
_cell_length_c                   13.534(3)
_cell_measurement_reflns_used    900
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.010
_cell_measurement_theta_min      1.775
_cell_volume                     7148(2)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'XS n/a (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rayonix SX165 CCD'
_diffrn_measurement_method       '/f scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7937
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            23575
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        28.439
_diffrn_reflns_theta_max         31.011
_diffrn_reflns_theta_min         1.979
_exptl_absorpt_coefficient_mu    1.827
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9159
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'XDS (Kabsh, 2010)'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_description       block
_exptl_crystal_F_000             3188
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.019
_refine_diff_density_min         -2.282
_refine_diff_density_rms         0.117
_refine_ls_abs_structure_details
;
 Flack x determined using 2311 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.031(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         8096
_refine_ls_number_restraints     107
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0645
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1278P)^2^+0.4734P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1705
_refine_ls_wR_factor_ref         0.1856
_reflns_Friedel_coverage         0.772
_reflns_Friedel_fraction_full    0.987
_reflns_Friedel_fraction_max     0.983
_reflns_number_gt                6404
_reflns_number_total             8096
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01482j2.cif
_cod_data_source_block           Ni-kmv85
_cod_depositor_comments
'Adding full bibliography for 7244095--7244098.cif.'
_cod_database_code               7244097
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.914
_shelx_estimated_absorpt_t_min   0.838
_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, All O(H,H) groups
2. Restrained distances
 N37-C38
 1.41 with sigma of 0.01
 C27A-C25 \\sim C25-C27B
 with sigma of 0.02
 C28B-C25 \\sim C25-C27A
 with sigma of 0.02
 C27B-C25 \\sim C25-C26A
 with sigma of 0.02
 C26A-C25 \\sim C25-C26B
 with sigma of 0.02
 C28A-C25 \\sim C25-C28B
 with sigma of 0.02
 C8A-C21A \\sim C8A-C21B
 with sigma of 0.02
 C21A-C8A \\sim C8A-C21B
 with sigma of 0.02
 C8B-C21B \\sim C8A-C21A
 with sigma of 0.02
 C23A-C21A \\sim C23B-C21B
 with sigma of 0.02
 C8A-C23A \\sim C8A-C23B
 with sigma of 0.04
 C21A-C24A \\sim C21B-C22B
 with sigma of 0.02
 C21A-C22A \\sim C21B-C24B
 with sigma of 0.02
 C24A-C22A \\sim C22B-C24B
 with sigma of 0.04
 C8A-C24A \\sim C8A-C22B
 with sigma of 0.04
 C8A-C22A \\sim C8A-C24B
 with sigma of 0.04
 C23A-C24A \\sim C23B-C22B
 with sigma of 0.04
 C23A-C22A \\sim C23B-C24B
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C26A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.1
Uanis(C7B) \\sim Ueq, Uanis(C7A) \\sim Ueq, Uanis(C8B) \\sim Ueq, Uanis(C8A)
\\sim Ueq, Uanis(C9B) \\sim Ueq, Uanis(C9A) \\sim Ueq, Uanis(C21B) \\sim Ueq,
Uanis(C24B) \\sim Ueq, Uanis(C22A) \\sim Ueq, Uanis(C23B) \\sim Ueq,
Uanis(C22B) \\sim Ueq, Uanis(C24A) \\sim Ueq, Uanis(C21A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C26A) = Uanis(C28B)
Uanis(C7A) = Uanis(C7B)
Uanis(C38) = Uanis(C39)
4. Others
 Sof(C27A)=Sof(H27D)=Sof(H27E)=Sof(H27F)=Sof(C28A)=Sof(H28D)=Sof(H28E)=
 Sof(H28F)=Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=1-FVAR(1)
 Sof(C26B)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C27B)=Sof(H27A)=Sof(H27B)=
 Sof(H27C)=Sof(C28B)=Sof(H28A)=Sof(H28B)=Sof(H28C)=FVAR(1)
 Sof(C23B)=Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(C21B)=Sof(C22B)=Sof(H22D)=
 Sof(H22E)=Sof(H22F)=Sof(C24B)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C7B)=Sof(H7B)=
 Sof(C8B)=Sof(C9B)=Sof(H9B)=1-FVAR(2)
 Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(C9A)=Sof(H9A)=Sof(C23A)=Sof(H23A)=Sof(H23B)=
 Sof(H23C)=Sof(C21A)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C22A)=
 Sof(H22A)=Sof(H22B)=Sof(H22C)=FVAR(2)
 Fixed Sof: H40(0.5) H41A(0.5) H41B(0.5)
5.a Free rotating group:
 O41(H41A,H41B), C6(C7B,C8B,C9B,C4,C5)
5.b Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B)
5.c Me refined with riding coordinates:
 C22A(H22A,H22B,H22C), C26A(H26D,H26E,H26F), C24B(H24D,H24E,H24F)
5.d Aromatic/amide H refined with riding coordinates:
 C18(H18), C16(H16), C7A(H7A), C9A(H9A), C36(H36), C7B(H7B), C9B(H9B)
5.e Tetrahedral OH refined with riding coordinates:
 O40(H40)
5.f Idealised Me refined as rotating group:
 C23A(H23A,H23B,H23C), C39(H39A,H39B,H39C), C26B(H26A,H26B,H26C), C27B(H27A,
 H27B,H27C), C28B(H28A,H28B,H28C), C24A(H24A,H24B,H24C), C38(H38A,H38B,H38C),
 C27A(H27D,H27E,H27F), C28A(H28D,H28E,H28F), C23B(H23D,H23E,H23F), C22B(H22D,
 H22E,H22F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              2440
_shelx_hkl_checksum              21590
_shelx_fab_checksum              66100
_olex2_submission_special_instructions 'No special instructions were received'