Single-Site Cobalt Catalysts at New Zr12(μ3-O)8(μ3-OH)8(μ2-OH)6 Metal-Organic Framework Nodes for Highly Active Hydrogenation of Nitroarenes, Nitriles, and Isocyanides.
Ji, Pengfei; Manna, Kuntal; Lin, Zekai; Feng, Xuanyu; Urban, Ania; Song, Yang; Lin, Wenbin; Journal of the American Chemical Society 139 (2017) 7004–7011; doi:10.1021/jacs.7b02394

data_4126027
_publ_section_title
;
 Single-Site Cobalt Catalysts at New Zr12(\m3-O)8(\m3-OH)8(\m2-OH)6
 Metal-Organic Framework Nodes for Highly Active Hydrogenation of
 Nitroarenes, Nitriles, and Isocyanides.
;
_journal_issue                   20
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7004
_journal_page_last               7011
_journal_paper_doi               10.1021/jacs.7b02394
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety
'C13.22 N1.41 O30.41 Zr6, C O2, C O1.5, 0.5(Cl)'
_chemical_formula_sum            'C15.21 Cl0.5 N1.4 O33.9 Zr6'
_chemical_formula_weight         1309.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_primary     direct
_audit_creation_date             2016-12-15
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.1600(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.4489(5)
_cell_length_b                   20.7494(9)
_cell_length_c                   30.7865(14)
_cell_measurement_reflns_used    9876
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.27
_cell_measurement_theta_min      2.24
_cell_volume                     7312.1(6)
_computing_cell_refinement       'SAINT V8.35A (?, 2016)'
_computing_data_reduction        'SAINT V8.35A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.767
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_unetI/netI     0.0704
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.767
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            39218
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.767
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         20.079
_diffrn_reflns_theta_min         1.141
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.432
_exptl_absorpt_correction_T_max  0.7445
_exptl_absorpt_correction_T_min  0.6299
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0851 before and 0.0580 after correction.
The Ratio of minimum to maximum transmission is 0.8461.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.380
_exptl_crystal_description       prism
_exptl_crystal_F_000             4966
_exptl_crystal_size_max          50.0
_exptl_crystal_size_mid          50.0
_exptl_crystal_size_min          50.0
_refine_diff_density_max         2.612
_refine_diff_density_min         -1.480
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         13490
_refine_ls_number_restraints     455
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0527
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0547P)^2^+72.1059P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1295
_refine_ls_wR_factor_ref         0.1428
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9189
_reflns_number_total             13490
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b02394_si_002.cif
_cod_data_source_block           cam-2_0m_a
_cod_depositor_comments          'Adding full bibliography for 4126027.cif.'
_cod_original_formula_sum        'C15.21 Cl0.50 N1.40 O33.90 Zr6'
_cod_database_code               4126027
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Restrained distances
 C4AA-O4AA
 1.3 with sigma of 0.02
 C9AA-N12 \\sim N12-C2
 with sigma of 0.02
2. Restrained planarity
 C11, N12, C2, O25
 with sigma of 0.1
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O4AA \\sim C4AA \\sim O24: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
5. Rigid body (RIGU) restrains
 O23, C8, N2, C5AA, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O23A, C12, O24
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O5AA, O6AA, C8AA, O1, C3, O2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O4AA, C4AA, O24
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O24A)=Sof(O23A)=Sof(C12)=1-FVAR(1)
 Sof(N2)=Sof(C5)=Sof(C8)=Sof(O23)=Sof(C5AA)=Sof(C4AA)=Sof(O4AA)=Sof(O24)=FVAR(1)
;
_olex2_submission_special_instructions 'No special instructions were received'