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_7126607
_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         'C66 H72 Cu4 N12 O12 S2, 4(Cl O4), 1.5(H2 O)'
_chemical_formula_sum            'C66 H75 Cl4 Cu4 N12 O29.5 S2'
_chemical_formula_weight         1968.46
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-03-30
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.0508(7)
_cell_length_b                   17.7526(7)
_cell_length_c                   24.8923(9)
_cell_measurement_reflns_used    9990
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      24.63
_cell_measurement_theta_min      2.44
_cell_volume                     7976.7(5)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            55448
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.021
_diffrn_reflns_theta_max         25.021
_diffrn_reflns_theta_min         1.609
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.329
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6131
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4028
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_exptl_transmission_factor_max   0.7452
_exptl_transmission_factor_min   0.6131
_refine_diff_density_max         1.776
_refine_diff_density_min         -1.603
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         7019
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0608
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0595P)^2^+58.7206P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1430
_refine_ls_wR_factor_ref         0.1605
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5267
_reflns_number_total             7019
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc02379e2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7126607--7126609.cif.'
_cod_original_formula_sum        'C66 H75 Cl4 Cu4 N12 O29.50 S2'
_cod_database_code               7126607
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H28A,H28B} of C28, {H22A,H22B} of C22, {H21A,H21B} of C21,
   {H20A,H20B} of C20, {H19A,H19B} of C19, {H13A,H13B} of C13, {H12A,H12B} of
  C12
 At 1.5 times of:
  All O(H) groups, {H2A,H2B} of C33, All O(H,H) groups
2. Restrained distances
 O2-H2B
 0.82 with sigma of 0.01
 O2-H2A
 0.82 with sigma of 0.01
 O17-H17A = O17-H17A_$1
 0.85 with sigma of 0.01
 H2B-H2A
 1.296731 with sigma of 0.02
 H17A_$1-H17A
 1.387434 with sigma of 0.02
3. Others
 Fixed Sof: O8(0.5) O10(0.5) O16(0.5) H16A(0.5) H16B(0.5) O17(0.25) H17A(0.5)
4.a Free rotating group:
 O16(H16A,H16B)
4.b Rotating group:
 O1(H1A,H1B)
4.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)
4.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), C24(H24), C25(H25), C26(H26), C27(H27), C30(H30), C31(H31),
  C32(H32), C33(H33)
;
_shelx_res_checksum              97661
_shelx_hkl_checksum              35285
_olex2_submission_special_instructions 'No special instructions were received'