Insights into the Structure‒Activity Relationships in Metal‒Organic Framework-Supported Nickel Catalysts for Ethylene Hydrogenation
Wang, Xingjie; Zhang, Xuan; Pandharkar, Riddhish; Lyu, Jiafei; Ray, Debmalya; Yang, Ying; Kato, Satoshi; Liu, Jian; Wasson, Megan C.; Islamoglu, Timur; Li, Zhong; Hupp, Joseph T.; Cramer, Christopher J.; Gagliardi, Laura; Farha, Omar K.; ACS Catalysis  (2020) 8995–9005; doi:10.1021/acscatal.0c01844

data_4517882
_publ_section_title
;
 Insights into the Structure--Activity Relationships in Metal--Organic
 Framework-Supported Nickel Catalysts for Ethylene Hydrogenation
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              8995
_journal_page_last               9005
_journal_paper_doi               10.1021/acscatal.0c01844
_journal_year                    2020
_chemical_formula_moiety         '0.04(C240 H168 Ni2.4 O96 Zr18)'
_chemical_formula_sum            'C10 H7 Ni0.1 O4 Zr0.75'
_chemical_formula_weight         265.44
_space_group_crystal_system      cubic
_space_group_IT_number           221
_space_group_name_Hall           '-P 4 2 3'
_space_group_name_H-M_alt        'P m -3 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2020-03-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            24
_cell_length_a                   28.2651(7)
_cell_length_b                   28.2651(7)
_cell_length_c                   28.2651(7)
_cell_measurement_reflns_used    9088
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      58.87
_cell_measurement_theta_min      3.50
_cell_volume                     22581.4(10)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      199.98
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.802
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 0.802
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            66461
_diffrn_reflns_point_group_measured_fraction_full 0.802
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         58.964
_diffrn_reflns_theta_min         1.563
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.894
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.5933
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0927 before and 0.0802 after correction. The Ratio of minimum to maximum transmission is 0.7894. The \l/2 correction factor is 0.0015.'
_exptl_crystal_density_diffrn    0.468
_exptl_crystal_description       cube
_exptl_crystal_F_000             3163
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.267
_refine_diff_density_min         -1.429
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.538
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     99
_refine_ls_number_reflns         3185
_refine_ls_number_restraints     145
_refine_ls_restrained_S_all      2.524
_refine_ls_R_factor_all          0.1675
_refine_ls_R_factor_gt           0.1542
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4908
_refine_ls_wR_factor_ref         0.5183
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2687
_reflns_number_total             3185
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c01844_si_006.cif
_cod_data_source_block           cu_xz119_0m
_cod_depositor_comments
'Adding full bibliography for 4517880--4517884.cif.'
_cod_original_cell_volume        22581.4(17)
_cod_original_formula_sum        'C10 H7 Ni0.10 O4 Zr0.75'
_cod_database_code               4517882
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.833
_shelx_estimated_absorpt_t_min   0.777
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Ni5-O4
 2.2 with sigma of 0.02
 C3-C2 \\sim C4-C3 \\sim C5-C4 \\sim C6-C5 \\sim C7-C6 \\sim C7-C2
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C2 \\sim C3 \\sim C4: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08
4. 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
5. Others
 Fixed Sof: H10A(0.5) H10B(0.5) H10C(0.5) Ni5(0.05)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C6(H6)
6.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C)
;
_olex2_submission_special_instructions 'No special instructions were received'