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_4130789
_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 O264 Zr52)'
_chemical_formula_sum            'C2.17 O0.45 Zr0.09'
_chemical_formula_weight         41.30
_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             2016-06-16
_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            587
_cell_length_a                   41.616(4)
_cell_length_b                   41.616(4)
_cell_length_c                   41.616(4)
_cell_measurement_reflns_used    9306
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      13.3079
_cell_measurement_theta_min      2.1672
_cell_volume                     72074(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 0.762
_diffrn_measured_fraction_theta_max 1.000
_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  0.1634
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 0.762
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            837497
_diffrn_reflns_point_group_measured_fraction_full 0.762
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         23.571
_diffrn_reflns_theta_min         1.094
_diffrn_source                   'synchrotron radiation'
_exptl_absorpt_coefficient_mu    0.210
_exptl_crystal_colour            bluish
_exptl_crystal_density_diffrn    0.559
_exptl_crystal_description       cube
_exptl_crystal_F_000             11824
_refine_diff_density_max         1.004
_refine_diff_density_min         -2.215
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         9409
_refine_ls_number_restraints     331
_refine_ls_restrained_S_all      1.224
_refine_ls_R_factor_all          0.1392
_refine_ls_R_factor_gt           0.1310
_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^)+(0.1948P)^2^+177.4415P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3539
_refine_ls_wR_factor_ref         0.3599
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8895
_reflns_number_total             9409
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b06759_si_004.cif
_cod_data_source_block           pom_3n-co_a
_cod_original_cell_volume        72073(21)
_cod_database_code               4130789
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Restrained planarity
 C27, C30, C2AA, C1AA, C26, C31
 with sigma of 0.1
 C23, C27, C26, C25, C19
 with sigma of 0.1
 C23, C26, C25, C24, C27, C19
 with sigma of 0.1
2. 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
3. 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
4.a Fitted hexagon refined as free rotating group:
 C9(C8,C11,C10,C13,C0AA), C32(C18,C12,C16,C33,C17)
;
_olex2_submission_special_instructions 'No special instructions were received'