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_7060104
_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         'C72 H60 N6 O20 Zr6, 2(Cl), 2(C3 H7 N O)'
_chemical_formula_sum            'C78 H74 Cl2 N8 O22 Zr6'
_chemical_formula_weight         2093.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 91.681(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   39.583(5)
_cell_length_b                   11.3619(16)
_cell_length_c                   19.236(3)
_cell_measurement_reflns_used    9816
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      57.000
_cell_measurement_theta_min      1.953
_cell_volume                     8647(2)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'OLEX2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2015b)'
_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 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '0.60\ % \ w and 0.6\ % \ f scans'
_diffrn_radiation_collimation    '0.5 mm double- pinhole'
_diffrn_radiation_detector       'Bruker D8 VENTURE'
_diffrn_radiation_monochromator  'equatorially mounted graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.1202
_diffrn_reflns_av_unetI/netI     0.1165
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            60829
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.159
_diffrn_reflns_theta_max         67.159
_diffrn_reflns_theta_min         3.351
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    6.911
_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    1.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4192
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.008
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1049
_refine_ls_number_reflns         14959
_refine_ls_number_restraints     234
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.1624
_refine_ls_R_factor_gt           0.0879
_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^)+(0.0802P)^2^+42.1006P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1809
_refine_ls_wR_factor_ref         0.2102
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8394
_reflns_number_total             14959
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj04576d2.cif
_cod_data_source_block           Zr-MC-3
_cod_depositor_comments
'Adding full bibliography for 7060103--7060105.cif.'
_cod_original_cell_volume        8648(2)
_cod_database_code               7060104
_shelx_shelxl_version_number     2018/3
_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, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N6-C77 = N6-C74 = N6-C30 = N8-C78 = N8-C76 = N8-C75
 1.5 with sigma of 0.01
3. Rigid body (RIGU) restrains
 C40, C63, C65, C67, C73
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C45, C52, C64, C69, C71
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C6, C18, C26, C33, C53
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C17, C39, C41, C51, C59
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C21, C25, C35, C46, C58
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C42, C43, C60, C68, C72
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O17, C30, N6, C74, C77
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C76, O18, C75, N8, C78
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4.a Aromatic/amide H refined with riding coordinates:
 O6(H6), O3(H3), O10(H10), O11(H11), O15(H15), O16(H16), C6(H6A), C7(H7),
 C8(H8), C11(H11A), C16(H16A), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21),
  C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C29(H29), C30(H30),
 C31(H31), C33(H33), C34(H34), C35(H35), 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), C56(H56), C57(H57), C58(H58),
  C59(H59), C60(H60), C61(H61), C62(H62), C63(H63), C64(H64), C65(H65),
 C66(H66), C67(H67), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72), C73(H73),
  C75(H75)
4.b Idealised Me refined as rotating group:
 C74(H74A,H74B,H74C), C76(H76A,H76B,H76C), C77(H77A,H77B,H77C), C78(H78A,H78B,
 H78C)
;
_shelx_res_checksum              53041
_shelx_fab_checksum              24974
_olex2_submission_special_instructions 'No special instructions were received'