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_7244113
_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 H62 Cl2 N6 Ni O20 Zr6, 2(Cl), 4(C4 H9 N O)'
_chemical_formula_sum            'C82 H98 Cl4 N10 Ni O24 Zr6'
_chemical_formula_weight         2355.53
_chemical_name_systematic        ZrMOF-Ni
_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             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                82.573(2)
_cell_angle_beta                 76.173(2)
_cell_angle_gamma                75.347(2)
_cell_formula_units_Z            1
_cell_length_a                   11.3213(6)
_cell_length_b                   12.5450(7)
_cell_length_c                   21.9866(13)
_cell_measurement_reflns_used    7881
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.12
_cell_measurement_theta_min      2.23
_cell_volume                     2925.7(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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_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  0.0824
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_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            74995
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.415
_diffrn_reflns_theta_min         2.208
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.823
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0111
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0722 before and 0.0678 after correction.
The Ratio of minimum to maximum transmission is 0.4022.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       block
_exptl_crystal_F_000             1188
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         11954
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0477
_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^)+(0.0894P)^2^+0.0121P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1317
_refine_ls_wR_factor_ref         0.1446
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9110
_reflns_number_total             11954
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01418h2.cif
_cod_data_source_block           2109222
_cod_depositor_comments
'Adding full bibliography for 7244112--7244113.cif.'
_cod_database_code               7244113
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.886
_shelx_estimated_absorpt_t_min   0.866
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00L(H00L), C00M(H00M), C00N(H00N), N00Q(H00Q), C00R(H00R), C00T(H00T),
 C00W(H00W), C00X(H00X), C00Z(H00Z), C012(H012), C013(H013), C015(H015),
 C017(H017), C018(H018), C019(H019), C01A(H01A), C01B(H01B), C01C(H01C),
 C01F(H01F), C01G(H01G), C01H(H01H), C01J(H01J), C01K(H01K), C01L(H01L),
 C01Q(H01Q), C01R(H01R), C01S(H01S), C01T(H01T)
2.b Idealised Me refined as rotating group:
 C00V(H00A,H00B,H00C), C016(H01D,H01E,H01I), C01E(H01M,H01N,H01O), C01I(H01P,
 H01U,H01V), C01P(H01W,H01X,H01Y), C01U(H01Z,H,HA)
;
_shelx_res_checksum              68661
_shelx_fab_checksum              30983
_olex2_submission_special_instructions 'No special instructions were received'