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_4130790
_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.
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_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 Hf52 O264)'
_chemical_formula_sum            'C1.25 Hf0.05 O0.26'
_chemical_formula_weight         28.33
_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'
_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            1016
_cell_length_a                   41.516(2)
_cell_length_b                   41.516(2)
_cell_length_c                   41.516(2)
_cell_measurement_reflns_used    9848
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      11.2934
_cell_measurement_theta_min      2.1724
_cell_volume                     71556(6)
_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      99.95
_diffrn_measured_fraction_theta_full 0.150
_diffrn_measured_fraction_theta_max 0.997
_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  0.1688
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 0.150
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            640669
_diffrn_reflns_point_group_measured_fraction_full 0.150
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         13.369
_diffrn_reflns_theta_min         0.638
_diffrn_source                   'synchrotron radiation'
_exptl_absorpt_coefficient_mu    0.424
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.668
_exptl_crystal_description       cube
_exptl_crystal_F_000             13488
_refine_diff_density_max         0.953
_refine_diff_density_min         -2.601
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.244
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         9175
_refine_ls_number_restraints     623
_refine_ls_restrained_S_all      1.253
_refine_ls_R_factor_all          0.1540
_refine_ls_R_factor_gt           0.1145
_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^)+(0.1367P)^2^+328.5184P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2758
_refine_ls_wR_factor_ref         0.3046
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7375
_reflns_number_total             9175
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b06759_si_003.cif
_cod_data_source_block           pm-3n-hf_a
_cod_original_cell_volume        71556(12)
_cod_database_code               4130790
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Restrained distances
 C1D-C8A
 1.468 with sigma of 0.02
 C8A-C58
 1.4 with sigma of 0.02
 C58-C12
 1.4 with sigma of 0.02
 C5A-C58
 2.425 with sigma of 0.02
 C12-C8A
 2.425 with sigma of 0.02
2. Restrained planarity
 C5B, C2B, C3B, C4B, C6B, C1B
 with sigma of 0.1
 C6B, C9B, C0, C5B
 with sigma of 0.1
 C1A, C3A, C5A, C4A, C2A, C0
 with sigma of 0.1
 C4A, C5A, C8A, C1D
 with sigma of 0.1
 C9B, C46, C19, C6B
 with sigma of 0.1
 C5A, C12, C58, C8A
 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
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
5. 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
6.a Fitted hexagon refined as free rotating group:
 C8(C9,C31,C2,C1AA,C0AA)
;
_olex2_submission_special_instructions 'No special instructions were received'