Modulation of hydrophilicity inside the cavity of molecular rectangles self-assembled under ambient conditions.
Khullar, Sadhika; Mandal, Sanjay K.; Chemical communications (Cambridge, England) 56 (2020) 7913–7916; doi:10.1039/d0cc02379e

data_7126608
_publ_section_title
;
 Modulation of hydrophilicity inside the cavity of molecular rectangles
 self-assembled under ambient conditions.
;
_journal_issue                   57
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7913
_journal_page_last               7916
_journal_paper_doi               10.1039/d0cc02379e
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         '2(C34 H38 Cu2 N6 O6 S), 4(Cl O4), 2(H2 O)'
_chemical_formula_sum            'C68 H80 Cl4 Cu4 N12 O30 S2'
_chemical_formula_weight         2005.52
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-03-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-01 deposited with the CCDC.	2020-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                73.309(9)
_cell_angle_beta                 78.299(12)
_cell_angle_gamma                63.132(9)
_cell_formula_units_Z            2
_cell_length_a                   15.352(5)
_cell_length_b                   15.546(5)
_cell_length_c                   19.838(6)
_cell_measurement_reflns_used    824
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      19.0209
_cell_measurement_theta_min      2.6609
_cell_volume                     4031(2)
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS, 2009)'
_computing_data_collection       'APEX2 (Bruker)'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.924
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0948
_diffrn_reflns_av_unetI/netI     0.2004
_diffrn_reflns_Laue_measured_fraction_full 0.924
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16452
_diffrn_reflns_point_group_measured_fraction_full 0.924
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        22.481
_diffrn_reflns_theta_max         22.481
_diffrn_reflns_theta_min         1.076
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.317
_exptl_absorpt_correction_T_max  0.7448
_exptl_absorpt_correction_T_min  0.5118
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_description       block
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.265
_refine_diff_density_min         -0.835
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     959
_refine_ls_number_reflns         9743
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1965
_refine_ls_R_factor_gt           0.0915
_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^)+(0.1044P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1972
_refine_ls_wR_factor_ref         0.2513
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4586
_reflns_number_total             9743
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc02379e2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7126607--7126609.cif.'
_cod_database_code               7126608
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.7448
_shelx_estimated_absorpt_t_min   0.5118
_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 O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O10) = Uanis(O12) = Uanis(O11) = Uanis(O9) = Uanis(O5) = Uanis(O6) =
Uanis(O3) = Uanis(O4)
Uanis(C29) = Uanis(C16) = Uanis(C18) = Uanis(C45) = Uanis(C48) = Uanis(C68) =
Uanis(C50) = Uanis(C55) = Uanis(C64) = Uanis(C39) = Uanis(C37) = Uanis(C59) =
Uanis(C42) = Uanis(C30)
Uanis(N4) = Uanis(N7) = Uanis(N12)
3.a Free rotating group:
 O29(H29C,H29D), O30(H30A,H30B)
3.b Rotating group:
 O1(H1A,H1B), O2(H2A,H2B), O7(H7A,H7B), O8(H8A,H8B)
3.c Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,
 H21B), C22(H22A,H22B), C28(H28A,H28B), C29(H29A,H29B), C46(H46A,H46B),
 C47(H47A,H47B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B),
  C57(H57A,H57B), C63(H63A,H63B)
3.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C15(H15), C16(H16),
 C17(H17), C18(H18), C23(H23), C24(H24), C25(H25), C26(H26), C31(H31), C32(H32),
  C33(H33), C34(H34), C37(H37), C38(H38), C41(H41), C42(H42), C43(H43),
 C44(H44), C49(H49), C50(H50), C51(H51), C52(H52), C59(H59), C60(H60), C61(H61),
  C62(H62), C65(H65), C66(H66), C67(H67), C68(H68)
;
_shelx_res_checksum              97916
_shelx_hkl_checksum              76239
_olex2_submission_special_instructions 'No special instructions were received'