A novel yttrium-based metal‒organic framework for the efficient solvent-free catalytic synthesis of cyanohydrin silyl ethers
Echenique-Errandonea, Estitxu; Pérez, Juana M.; Rojas, Sara; Cepeda, Javier; Seco, José M.; Fernández, Ignacio; Rodríguez-Diéguez, Antonio; Dalton Transactions 50 (2021) 11720–11724; doi:10.1039/D1DT01953H

data_7708077
_publ_section_title
;
 A novel yttrium-based metal--organic framework for the efficient
 solvent-free catalytic synthesis of cyanohydrin silyl ethers
;
_journal_issue                   34
_journal_name_full               'Dalton Transactions'
_journal_page_first              11720
_journal_page_last               11724
_journal_paper_doi               10.1039/D1DT01953H
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C51 H54 N9 O24 Y5, [H2O]'
_chemical_formula_sum            'C51 H56 N9 O25 Y5'
_chemical_formula_weight         1639.59
_chemical_name_systematic
Poly{[hexa(mu3-3-amino-4-hydroxybenzoate-k2O,O':kO'':k2N,O''')tri(mu3-hydroxide-kO:kO':kO'')tri(dimethylformamide-kO)pentayttrium(III)]pentahydrate}
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-07-22
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6380)
;
_audit_update_record
;
2021-07-30 deposited with the CCDC.	2021-08-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   14.730(3)
_cell_length_b                   14.730
_cell_length_c                   17.616(5)
_cell_measurement_reflns_used    12689
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.358
_cell_measurement_theta_min      2.312
_cell_volume                     3310.1(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker Venture'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0933
_diffrn_reflns_av_unetI/netI     0.0922
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12673
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        23.358
_diffrn_reflns_theta_max         23.358
_diffrn_reflns_theta_min         2.766
_exptl_absorpt_coefficient_mu    4.417
_exptl_absorpt_correction_T_max  0.533
_exptl_absorpt_correction_T_min  0.236
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
SADABS, Program for Empirical Adsorption Correction, 
Institute for Inorganic Chemistry, University of Gottingen: Germany, 
1996Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_density_method    none
_exptl_crystal_description       needle
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.358
_refine_diff_density_min         -0.960
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         1667
_refine_ls_number_restraints     130
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0542P)^2^+12.5788P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1005
_refine_ls_wR_factor_ref         0.1151
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1260
_reflns_number_total             1667
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01953h2.cif
_cod_data_source_block           compound1
_cod_depositor_comments          'Adding full bibliography for 7708077.cif.'
_cod_original_cell_volume        3310.1(17)
_cod_database_code               7708077
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.692
_shelx_estimated_absorpt_t_min   0.159
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Others
 Fixed Sof: H2DA(0.5) H2DB(0.5) H2DC(0.5) H3DA(0.5) H3DB(0.5) H3DC(0.5)
4.a Everything fixed:
 H2DA, H2DB, H2DC, H3DA, H3DB, H3DC
4.b Ternary CH refined with riding coordinates:
 O1H(H1H)
4.c Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B)
4.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7), C1D(H1D)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'