One-step synthesis of pure-phase amino-functionalized zirconium-based capsule ZrC-1-NH2 for photocatalytic degradation of tetracycline
Xu, Ting-Ting; Wei, De-Sheng; Li, Shuang-Bao; Zhang, Yu-Teng; Lv, Nan; CrystEngComm 26 (2024) 5431–5439; doi:10.1039/D4CE00721B

data_7249249
_publ_section_title
;
 One-step synthesis of pure-phase amino-functionalized zirconium-based
 capsule ZrC-1-NH2 for photocatalytic degradation of tetracycline
;
_journal_issue                   38
_journal_name_full               CrystEngComm
_journal_page_first              5431
_journal_page_last               5439
_journal_paper_doi               10.1039/D4CE00721B
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C54 H46 N3 O20 Zr6, 2(Cl), 0.5(H4 O2)'
_chemical_formula_sum            'C54 H48 Cl2 N3 O21 Zr6'
_chemical_formula_weight         1693.17
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-07-16
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-07-16 deposited with the CCDC.	2024-08-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.8615(12)
_cell_length_b                   17.7218(10)
_cell_length_c                   17.2448(12)
_cell_measurement_reflns_used    9176
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      56.81
_cell_measurement_theta_min      2.91
_cell_volume                     6069.9(7)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.737
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.737
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6307
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.737
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         68.644
_diffrn_reflns_theta_min         2.907
_diffrn_source_current           2.86
_diffrn_source_power             0.19977099999999998
_diffrn_source_voltage           69.85
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.389
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1779 before and 0.0840 after correction.
 
For component 2:
 wR2(int) was 0.1831 before and 0.0833 after correction.
 
For component 3:
 wR2(int) was 0.1972 before and 0.0905 after correction.
 The Ratio of minimum to maximum transmission is 0.57.

Final HKLF 4 output contains 81481 reflections, Rint = 0.1048
 (40504 with I > 3sig(I), Rint = 0.0934)
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.853
_exptl_crystal_description       block
_exptl_crystal_F_000             3340
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.760
_refine_diff_density_min         -1.356
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         3322
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0680
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1199P)^2^+54.8467P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1991
_refine_ls_wR_factor_ref         0.2027
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3024
_reflns_number_total             3322
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00721b2.cif
_cod_data_source_block           ZrC-1-NH2
_cod_depositor_comments          'Adding full bibliography for 7249249.cif.'
_cod_database_code               7249249
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.377
_shelx_estimated_absorpt_t_min   0.347
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 H6-Zr2
 2.82 with sigma of 0.02
 H6-Zr1
 2.82 with sigma of 0.02
 H4-Zr2
 2.8 with sigma of 0.02
 C4_$1-C1_$1
 1.63 with sigma of 0.02
 C4-C1 = C6-C5
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C15 \\sim C12 \\sim C14 \\sim C13 \\sim C11 \\sim C9 \\sim C10: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N2) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(N2) \\sim
Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O0AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: H4(0.5) N1(0.5) H1A(0.5) H1B(0.5) N2(0.25) H2A(0.25) H2B(0.25)
 Cl2(0.25) H0AA(0.25) H0AB(0.25)
 Fixed X: O4(0.151641)
 Fixed Y: Zr2(0.59481) H6(0.488629)
 Fixed Z: O6(0.33837)
5.a Riding coordinates:
 O0AA(H0AA,H0AB)
5.b Free rotating group:
 O4(H4)
5.c Ternary CH refined with riding coordinates:
 C8(H8), C9(H9), C10(H10)
5.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15)
5.e Fitted pentagon refined as free rotating group:
 C11(C12,C13,C14,C15)
5.f X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B)
;
_shelx_res_checksum              55043
_shelx_hkl_checksum              96425
_olex2_submission_special_instructions 'No special instructions were received'