Single-Site Cobalt Catalysts at New Zr8(μ2-O)8(μ2-OH)4 Metal-Organic Framework Nodes for Highly Active Hydrogenation of Alkenes, Imines, Carbonyls, and Heterocycles.
Ji, Pengfei; Manna, Kuntal; Lin, Zekai; Urban, Ania; Greene, Francis X.; Lan, Guangxu; Lin, Wenbin; Journal of the American Chemical Society 138 (2016) 12234–12242; doi:10.1021/jacs.6b06759

data_4130788
_publ_section_title
;
 Single-Site Cobalt Catalysts at New Zr8(\m2-O)8(\m2-OH)4 Metal-Organic
 Framework Nodes for Highly Active Hydrogenation of Alkenes, Imines,
 Carbonyls, and Heterocycles.
;
_journal_issue                   37
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12234
_journal_page_last               12242
_journal_paper_doi               10.1021/jacs.6b06759
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         '0(C1272 H576 O264 Zr52)'
_chemical_formula_sum            'C1.17 H0.53 O0.24 Zr0.05'
_chemical_formula_weight         22.90
_space_group_crystal_system      cubic
_space_group_IT_number           223
_space_group_name_Hall           '-P 4n 2 3'
_space_group_name_H-M_alt        'P m -3 n'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-06-20
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1084
_cell_length_a                   41.512(4)
_cell_length_b                   41.512(4)
_cell_length_c                   41.512(4)
_cell_measurement_reflns_used    3755
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      9.1658
_cell_measurement_theta_min      2.2463
_cell_volume                     71535(12)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'synchrotron, beamline 15-ID, APEX2 detector'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_type           'synchrotron radiation'
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.2571
_diffrn_reflns_av_unetI/netI     0.1955
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            419963
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.396
_diffrn_reflns_theta_min         1.097
_diffrn_source                   'synchrotron radiation'
_exptl_absorpt_coefficient_mu    0.212
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.576
_exptl_crystal_description       cube
_exptl_crystal_F_000             12400
_refine_diff_density_max         0.667
_refine_diff_density_min         -1.459
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         12692
_refine_ls_number_restraints     621
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.2586
_refine_ls_R_factor_gt           0.1276
_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^)+(0.1719P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3136
_refine_ls_wR_factor_ref         0.3628
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6116
_reflns_number_total             12692
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b06759_si_002.cif
_cod_data_source_block           final
_cod_original_cell_volume        71534(19)
_cod_database_code               4130788
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C8-C20
 1.468 with sigma of 0.02
3. Restrained planarity
 C3, C10, C5AA, C8AA, C4
 with sigma of 0.1
 C1BA, C6AA, C7, C2AA, C9, C12
 with sigma of 0.1
 C00B, C3AA, C00G, C00J
 with sigma of 0.1
 C2, C20, C9AA, C19
 with sigma of 0.1
 C0AA, C13, C17, C1
 with sigma of 0.1
4. 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
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
6. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7.a Aromatic/amide H refined with riding coordinates:
 C00G(H00G), C3AA(H3AA), C4(H4), C8AA(H8AA), C10(H10), C7AA(H7AA), C6AA(H6AA),
 C7(H7), C9(H9), C12(H12), C9AA(H9AA), C19(H19)
7.b Fitted hexagon refined as free rotating group:
 C3(C4,C8AA,C5AA,C10,C7AA), C1BA(C6AA,C7,C2AA,C9,C12)
;
_olex2_submission_special_instructions 'No special instructions were received'