Self-assembly of zirconocene-based metal‒organic capsules: the structure, luminescence sensing of Fe3+ and iodine capture
Chen, Siyuan; Cheng, Shuangjing; Zhao, Liang; Sun, Chunyi; Qin, Chao; Su, Zhongmin; New Journal of Chemistry 44 (2020) 21255–21260; doi:10.1039/D0NJ04576D

data_7060103
_publ_section_title
;
 Self-assembly of zirconocene-based metal--organic capsules: the
 structure, luminescence sensing of Fe3+ and iodine capture
;
_journal_issue                   48
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              21255
_journal_page_last               21260
_journal_paper_doi               10.1039/D0NJ04576D
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C54 H48 O20 Zr6, 2(Cl), C4 H9 N O, H O'
_chemical_formula_sum            'C58 H59 Cl2 N O22 Zr6'
_chemical_formula_weight         1740.28
_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             2020-08-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-08-21 deposited with the CCDC.	2020-11-17 downloaded from the CCDC.
;
_cell_angle_alpha                72.965(2)
_cell_angle_beta                 80.879(3)
_cell_angle_gamma                80.069(3)
_cell_formula_units_Z            2
_cell_length_a                   14.7990(8)
_cell_length_b                   16.2691(10)
_cell_length_c                   17.0541(9)
_cell_measurement_reflns_used    9962
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.000
_cell_measurement_theta_min      1.953
_cell_volume                     3841.6(4)
_computing_cell_refinement       'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      173.02
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker D8 VENTURE'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '0.5\% \w and 0.5\% \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_detector       'Bruker D8 VENTURE'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.1279
_diffrn_reflns_av_unetI/netI     0.0960
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            66772
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.113
_diffrn_reflns_theta_max         25.113
_diffrn_reflns_theta_min         2.632
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.917
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.107
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     760
_refine_ls_number_reflns         13631
_refine_ls_number_restraints     213
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1459
_refine_ls_R_factor_gt           0.0630
_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^)+(0.0760P)^2^+27.9275P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1449
_refine_ls_wR_factor_ref         0.1963
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7367
_reflns_number_total             13631
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj04576d2.cif
_cod_data_source_block           Zr-MC-1
_cod_depositor_comments
'Adding full bibliography for 7060103--7060105.cif.'
_cod_database_code               7060103
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.54
_shelx_estimated_absorpt_t_min   0.21
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H2 of O2, H3 of O3, H4 of O4, H5 of O5, H6 of O6, H15 of O15
 At 1.5 times of:
  All C(H,H,H) groups, H22 of O22
2. Rigid body (RIGU) restrains
 C30, C31, C32, C33, C34
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C40, C41, C42, C43, C44
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C50, C51, C52, C53, C54
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C35, C36, C37, C38, C39
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C45, C46, C47, C48, C49
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C5, C6, C7, C8, C9
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N1, O21, C56, C57, C55, C58
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3.a Free rotating group:
 O22(H22)
3.b :
 C5(C6,C7,C8,C9), C30(C31,C32,C33,C34), C35(C36,C37,C38,C39), C40(C41,C42,C43,
 C44), C45(C46,C47,C48,C49), C50(C51,C52,C53,C54)
3.c Aromatic/amide H refined with riding coordinates:
 O2(H2), O3(H3), O4(H4), O5(H5), O6(H6), O15(H15), C2(H2A), C3(H3A), C5(H5A),
 C6(H6A), C7(H7), C8(H8), C9(H9), C10(H10), C15(H15A), C16(H16), C20(H20),
 C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31),
  C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38),
 C39(H39), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46),
  C47(H47), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54)
3.d Idealised Me refined as rotating group:
 C55(H55A,H55B,H55C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C)
;
_shelx_res_checksum              38491
_shelx_fab_checksum              15142
_olex2_submission_special_instructions 'No special instructions were received'