Synthesis of zirconium-based metal–organic frameworks with iron(ii) clathrochelate ligands
Shetty, Suchetha; Idrees, Karam B.; Xie, Haomiao; Alameddine, Bassam; Farha, Omar K.; CrystEngComm 25 (2023) 1550–1555; doi:10.1039/D2CE01686A

data_7246245
_publ_section_title
;
 Synthesis of zirconium-based metal--organic frameworks with iron(ii)
 clathrochelate ligands
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              1550
_journal_page_last               1555
_journal_paper_doi               10.1039/D2CE01686A
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C120 H48 B12 Fe6 N36 O68 Zr6'
_chemical_formula_sum            'C120 H48 B12 Fe6 N36 O68 Zr6'
_chemical_formula_weight         4094.08
_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_Hall           '-F 4 2 3'
_space_group_name_H-M_alt        'F m -3 m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-11-12
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-12-06 deposited with the CCDC.	2023-02-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   37.5848(3)
_cell_length_b                   37.5848(3)
_cell_length_c                   37.5848(3)
_cell_measurement_reflns_used    5258
_cell_measurement_temperature    200.01(10)
_cell_measurement_theta_max      73.7070
_cell_measurement_theta_min      3.8950
_cell_volume                     53092.9(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -27.00  19.00   0.50   40.00    --   47.48 -20.00 -87.00   92
  2  \w     42.00 108.00   0.50  170.00    --  113.25-108.00  10.00  132
  3  \w    -27.00  17.00   0.50   40.00    --   47.48 -19.00  60.00   88
  4  \w    -75.00 -33.00   0.50  170.00    -- -106.00  61.00   0.00   84
  5  \w     42.00  82.00   0.50  170.00    --  113.25 -67.00-171.00   80
  6  \w     42.00  71.00   0.50  170.00    --  113.25 -61.00 150.00   58
  7  \w   -120.00 -95.00   0.50   40.00    --  -47.48 -62.00  43.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0079383000
_diffrn_orient_matrix_UB_12      0.0113112000
_diffrn_orient_matrix_UB_13      0.0385968000
_diffrn_orient_matrix_UB_21      0.0305000000
_diffrn_orient_matrix_UB_22      -0.0273548000
_diffrn_orient_matrix_UB_23      0.0017362000
_diffrn_orient_matrix_UB_31      0.0262037000
_diffrn_orient_matrix_UB_32      0.0283653000
_diffrn_orient_matrix_UB_33      -0.0136732000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0909
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            26210
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.371
_diffrn_reflns_theta_min         3.901
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.471
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67255
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.121a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.512
_exptl_crystal_description       block
_exptl_crystal_F_000             8080
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.667
_refine_diff_density_min         -0.935
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         2811
_refine_ls_number_restraints     137
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0793
_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^)+(0.1685P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2163
_refine_ls_wR_factor_ref         0.2257
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2246
_reflns_number_total             2811
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01686a2.cif
_cod_data_source_block           zr-kwait-def-200k_auto
_cod_depositor_comments          'Adding full bibliography for 7246245.cif.'
_cod_original_cell_volume        53092.7(14)
_cod_database_code               7246245
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Zr Fe N C O'
_shelx_estimated_absorpt_t_max   0.708
_shelx_estimated_absorpt_t_min   0.638
_olex2_refinement_description
;
1. Restrained distances
 C3-C2 = C4-C3 = C4-C5 = C4_$1-C5 = C4-C3 = C3_$1-C2
 1.39 with sigma of 0.01
 C4_$1-C3 = C5-C2 = C4-C3_$1
 2.78 with sigma of 0.02
 C6-C6_$4
 1.38 with sigma of 0.01
 Fe1-N3 \\sim Fe1-N2 \\sim Fe1-N1
 with sigma of 0.01
 C7-C7_$4 \\sim C8-C8_$4 \\sim C6-C6_$4
 with sigma of 0.01
2. Rigid bond restraints
 O5, Zr1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim Fe1 \\sim O4 \\sim O5 \\sim B1
\\sim C6 \\sim C7 \\sim C8 \\sim N1 \\sim N2 \\sim N3 \\sim O1 \\sim O2 \\sim
O3: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A
Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Others
 Fixed Sof: B1(0.0625) C6(0.25) C7(0.25) C8(0.25) N1(0.25) N2(0.25) N3(0.25)
 O1(0.25) O2(0.25) O3(0.25)
5.a Free rotating group:
 B1(C6,C7,C8,N1,N2,N3,O1,O2,O3)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              76348
_shelx_hkl_checksum              53901
_shelx_fab_checksum              27833
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.561
_oxdiff_exptl_absorpt_empirical_full_min 0.510