Two-Dimensional Zr/Hf-Hydroxamate Metal-Organic Frameworks
Lai, Qiuxue; Chu, Zhao-Qin; Xiao, Xinyi; Dai, Dejun; Song, Ting; Luo, Tian-Yi; Tang, Wenlei; Feng, Xuan; Zhang, Zhiyuan; Li, Tao; Xiao, Hai; Su, Jing; Liu, Chong; Chemical Communications  (2022) –; doi:10.1039/D2CC00213B

data_7129623
_publ_section_title
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 Two-Dimensional Zr/Hf-Hydroxamate Metal-Organic Frameworks
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC00213B
_journal_year                    2022
_chemical_formula_moiety         '0.33(C48 H36 N12 O24 Zr3)'
_chemical_formula_sum            'C16 H12 N4 O8 Zr'
_chemical_formula_weight         479.52
_space_group_crystal_system      hexagonal
_space_group_IT_number           191
_space_group_name_Hall           '-P 6 2'
_space_group_name_H-M_alt        'P 6/m m m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-07-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-12-08 deposited with the CCDC.	2022-01-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   23.168(2)
_cell_length_b                   23.168(2)
_cell_length_c                   8.0801(11)
_cell_measurement_reflns_used    4098
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      23.40
_cell_measurement_theta_min      2.69
_cell_volume                     3756.0(7)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1500
_diffrn_reflns_av_unetI/netI     0.0507
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            36009
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.496
_diffrn_reflns_theta_min         2.030
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.240
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5888
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1032 before and 0.0853 after correction. The Ratio of minimum to maximum transmission is 0.7897. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.636
_exptl_crystal_description       block
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.664
_refine_diff_density_min         -1.374
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     64
_refine_ls_number_reflns         1724
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.1019
_refine_ls_R_factor_gt           0.0892
_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^)+(0.1742P)^2^+2.6618P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2487
_refine_ls_wR_factor_ref         0.2633
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1315
_reflns_number_total             1724
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00213b2.cif
_cod_data_source_block           SUM-1Zr
_cod_original_cell_volume        3756.1(9)
_cod_database_code               7129623
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.974
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Others
 Fixed Sof: O2(0.5) O1(0.5) N1(0.5) H1(0.5) C3(0.5) H3(0.5) C4(0.5) H4(0.5)
 C1(0.5)
3.a Ternary CH refined with riding coordinates:
 N1(H1)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4)
;
_olex2_submission_special_instructions 'No special instructions were received'