Stepwise synthesis of Zr-based metal–organic frameworks: incorporating a trinuclear zirconocene-based metallo-pyridine ligand
Zhu, Juan; Liu, Zhao-Yang; Li, Shuang-bao; Huang, He; Jiang, Bao-Xu; Zhang, Yu-Teng; CrystEngComm 24 (2022) 475–478; doi:10.1039/D1CE01418H

data_7244112
_publ_section_title
;
 Stepwise synthesis of Zr-based metal--organic frameworks: incorporating a
 trinuclear zirconocene-based metallo-pyridine ligand
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              475
_journal_page_last               478
_journal_paper_doi               10.1039/D1CE01418H
_journal_volume                  24
_journal_year                    2022
_chemical_formula_moiety
'C66 H60 Cl2 Co N6 O20 Zr6, 4(C4 H9 N O), 2(Cl)'
_chemical_formula_sum            'C82 H96 Cl4 Co N10 O24 Zr6'
_chemical_formula_weight         2353.73
_chemical_name_systematic        ZrMOF-Co
_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     iterative
_audit_creation_date             2021-10-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-11-24 deposited with the CCDC.	2021-12-23 downloaded from the CCDC.
;
_cell_angle_alpha                82.236(2)
_cell_angle_beta                 76.045(2)
_cell_angle_gamma                75.545(2)
_cell_formula_units_Z            1
_cell_length_a                   11.3034(6)
_cell_length_b                   12.7188(6)
_cell_length_c                   21.9772(12)
_cell_measurement_reflns_used    8784
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.15
_cell_measurement_theta_min      2.23
_cell_volume                     2959.8(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0976
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            91732
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.403
_diffrn_reflns_theta_min         2.226
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.795
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0109
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0822 before and 0.0761 after correction.
The Ratio of minimum to maximum transmission is 0.3949.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_description       block
_exptl_crystal_F_000             1185
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.830
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         12090
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0526
_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^)+(0.0846P)^2^+3.4645P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1410
_refine_ls_wR_factor_ref         0.1565
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9099
_reflns_number_total             12090
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01418h2.cif
_cod_data_source_block           2109221
_cod_depositor_comments
'Adding full bibliography for 7244112--7244113.cif.'
_cod_database_code               7244112
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.883
_shelx_estimated_absorpt_t_min   0.864
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C15(H15), C14(H14), C13(H13), C12(H12), C25(H25), C26(H26),
 C27(H27), C24(H24), C21(H21), C20(H20), C19(H19), C18(H18), C5(H5), C1(H1A),
 C2(H2A), C3(H3A), C4(H4), C30(H30), C31(H31), C8(H8), C9(H9), C10(H10), C6(H6),
  C7(H7), C32(H32), C33(H33)
2.b Fitted hexagon refined as free rotating group:
 C25(N3,C26,C27,C23,C24), C17(C21,C20,N1,C19,C18)
2.c Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C38(H38A,H38B,H38C), C41(H41A,H41B,H41C), C37(H37A,H37B,
 H37C), C36(H36A,H36B,H36C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              33091
_shelx_fab_checksum              36285
_olex2_submission_special_instructions 'No special instructions were received'