A Metal–Organic Framework-Supported Dinuclear Iron Catalyst for Hydroboration of Carbonyl Compounds
Zhu, Yi-Jie; Wang, Jun-Jie; Li, Jun-Yu; Zhang, Teng; Dalton Transactions  (2023) –; doi:10.1039/D3DT01109G

data_7712947
_publ_section_title
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 A Metal--Organic Framework-Supported Dinuclear Iron Catalyst for
 Hydroboration of Carbonyl Compounds
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01109G
_journal_year                    2023
_chemical_formula_moiety         'C60 H48 N16 O32 Zr6, 24[C3H7NO]'
_chemical_formula_sum            'C132 H216 N40 O56 Zr6'
_chemical_formula_weight         3806.76
_space_group_crystal_system      orthorhombic
_space_group_IT_number           58
_space_group_name_Hall           '-P 2 2n'
_space_group_name_H-M_alt        'P n n m'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-05-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-05-03 deposited with the CCDC.	2023-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   31.786(3)
_cell_length_b                   13.9537(15)
_cell_length_c                   24.406(2)
_cell_measurement_reflns_used    3073
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21.472
_cell_measurement_theta_min      2.561
_cell_volume                     10824.8(18)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.03
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  Bruker
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1434
_diffrn_reflns_av_unetI/netI     0.1067
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            35104
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        23.256
_diffrn_reflns_theta_max         23.256
_diffrn_reflns_theta_min         2.554
_exptl_absorpt_coefficient_mu    0.352
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.5316
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0870 before and 0.0714 after correction.
The Ratio of minimum to maximum transmission is 0.7137.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_description       block
_exptl_crystal_F_000             3952
_refine_diff_density_max         0.571
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         7973
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1009
_refine_ls_R_factor_gt           0.0688
_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^)+(0.1188P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1902
_refine_ls_wR_factor_ref         0.2117
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4748
_reflns_number_total             7973
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01109g2.cif
_cod_data_source_block           mo_zyj1_0ma
_cod_database_code               7712947
_shelx_shelxl_version_number     2018/3
_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 O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N2) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C7) \\sim
Ueq, Uanis(N1) \\sim Ueq, Uanis(N4) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
3. Others
 Fixed Sof: H2A(0.5) H3C(0.5)
4.a Rotating group:
 O3(H3A,H3B), O7(H7A,H7B)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C10(H10), C2(H2), C5(H5), C11(H11), C3(H3), N2(H2A), N3(H3C)
4.c Fitted hexagon refined as free rotating group:
 C4(C6,C8,C10,N1,C12), C15(C2,N4,C9,C5,C11)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 1898 electrons were 
found in a volume of 8056\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
24[C3H7NO] per Formula Unit 
which account for 1920 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              69277
_shelx_fab_checksum              36320
_olex2_submission_special_instructions 'No special instructions were received'