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_7244095
_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_formula_moiety         'C96 H104 Co8 O42 S8, 2(C3 H7 N O)'
_chemical_formula_sum            'C102 H118 Co8 N2 O44 S8'
_chemical_formula_weight         2803.90
_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_block_doi                 10.5517/ccdc.csd.cc2911q4
_audit_creation_date             2020-03-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-10-17 deposited with the CCDC.	2021-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                84.09(3)
_cell_angle_beta                 84.24(3)
_cell_angle_gamma                64.85(3)
_cell_formula_units_Z            1
_cell_length_a                   12.638(3)
_cell_length_b                   13.524(3)
_cell_length_c                   21.208(4)
_cell_measurement_reflns_used    1000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      3.284
_cell_measurement_theta_min      30.955
_cell_volume                     3257.3(15)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Rayonix SX165 CCD'
_diffrn_measurement_method       '/f scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7927
_diffrn_reflns_av_R_equivalents  0.0703
_diffrn_reflns_av_unetI/netI     0.0683
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            49598
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        28.782
_diffrn_reflns_theta_max         30.955
_diffrn_reflns_theta_min         3.284
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.623
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'XDS (Kabsh, 2010)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.147
_refine_diff_density_min         -1.608
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     694
_refine_ls_number_reflns         13943
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1267
_refine_ls_R_factor_gt           0.1101
_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^)+(0.1795P)^2^+15.0685P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2865
_refine_ls_wR_factor_ref         0.3052
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10952
_reflns_number_total             13943
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01482j2.cif
_cod_data_source_block           kmv86
_cod_depositor_comments
'Adding full bibliography for 7244095--7244098.cif.'
_cod_original_cell_volume        3257.3(14)
_cod_database_code               7244095
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.737
_shelx_estimated_absorpt_t_min   0.542
_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. Restrained distances
 C40A-C37 \\sim C37-C39B
 with sigma of 0.02
 C39B-C37 \\sim C37-C39A
 with sigma of 0.02
 C39A-C37 \\sim C37-C38B
 with sigma of 0.02
 C38A-C37 \\sim C37-C40B
 with sigma of 0.02
 C40B-C37 \\sim C37-C40A
 with sigma of 0.02
 C8-N1 \\sim N4-C1B
 with sigma of 0.02
 C1A-N1 \\sim N1-N4
 with sigma of 0.02
 C1C-N1 \\sim N4-C15
 with sigma of 0.02
 C29-C31 \\sim C33-C36
 with sigma of 0.02
 C29-C30 \\sim C33-C35
 with sigma of 0.02
 C29-C32 \\sim C33-C34
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.1
Uanis(C34) = Uanis(C30)
Uanis(C35) = Uanis(C32)
Uanis(C36) = Uanis(C31)
Uanis(C33) = Uanis(C29)
Uanis(C39A) = Uanis(C39B) = Uanis(C40A) = Uanis(C40B) = Uanis(C38A) =
Uanis(C38B)
Uanis(N1) = Uanis(N4) = Uanis(C1C) = Uanis(C15) = Uanis(C1B) = Uanis(C1A) =
Uanis(C1) = Uanis(O1) = Uanis(C8)
4. Others
 Sof(C40B)=Sof(H40A)=Sof(H40B)=Sof(H40C)=Sof(C38B)=Sof(H38A)=Sof(H38B)=
 Sof(H38C)=Sof(C39B)=Sof(H39D)=Sof(H39E)=Sof(H39F)=1-FVAR(1)
 Sof(C40A)=Sof(H40D)=Sof(H40E)=Sof(H40F)=Sof(C39A)=Sof(H39A)=Sof(H39B)=
 Sof(H39C)=Sof(C38A)=Sof(H38D)=Sof(H38E)=Sof(H38F)=FVAR(1)
 Sof(C1A)=Sof(H1A)=Sof(N1)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=Sof(C1C)=
 Sof(H1CA)=Sof(H1CB)=Sof(H1CC)=1-FVAR(2)
 Sof(C1)=Sof(H1)=Sof(N4)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C15)=Sof(H15A)=
 Sof(H15B)=Sof(H15C)=FVAR(2)
5.a Free rotating group:
 C14(C9,C10,C11,C12,C13), C1(N4,C8,C15), O1(C1A,N1,C1B,C1C)
5.b Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C52(H52A,H52B), C61(H61A,H61B), C62(H62A,H62B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C10(H10), C12(H12), C17(H17), C19(H19), C24(H24), C26(H26),
 C1(H1), C1A(H1A)
5.d Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C40B(H40A,H40B,
 H40C), C40A(H40D,H40E,H40F), C38B(H38A,H38B,H38C), C42(H42A,H42B,H42C),
 C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C39A(H39A,H39B,H39C), C39B(H39D,H39E,
 H39F), C38A(H38D,H38E,H38F), C8(H8A,H8B,H8C), C15(H15A,H15B,H15C), C1B(H1BA,
 H1BB,H1BC), C1C(H1CA,H1CB,H1CC), C35(H35A,H35B,H35C), C34(H34A,H34B,H34C),
 C36(H36A,H36B,H36C)
;
_shelx_res_checksum              62806
_shelx_hkl_checksum              12814
_shelx_fab_checksum              59014
_olex2_submission_special_instructions 'No special instructions were received'