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_4517880
_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         '0.17(C264 H132 Ni2.64 O102 Zr18)'
_chemical_formula_sum            'C44.33 H22 Ni0.44 O17 Zr3'
_chemical_formula_weight         1126.11
_space_group_crystal_system      hexagonal
_space_group_IT_number           191
_space_group_name_Hall           '-P 6 2'
_space_group_name_H-M_alt        'P 6/m m m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-03-02
_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                120
_cell_formula_units_Z            6
_cell_length_a                   39.4522(6)
_cell_length_b                   39.4522(6)
_cell_length_c                   16.5041(3)
_cell_measurement_reflns_used    9796
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      49.74
_cell_measurement_theta_min      5.96
_cell_volume                     22246.7(6)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.570
_diffrn_measured_fraction_theta_max 0.991
_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  0.0619
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.570
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            52289
_diffrn_reflns_point_group_measured_fraction_full 0.570
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         49.780
_diffrn_reflns_theta_min         5.812
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.946
_exptl_absorpt_correction_T_max  0.7498
_exptl_absorpt_correction_T_min  0.6517
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0631 before and 0.0519 after correction. The Ratio of minimum to maximum transmission is 0.8692. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.504
_exptl_crystal_description       rod
_exptl_crystal_F_000             3338
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.996
_refine_diff_density_min         -0.930
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         4275
_refine_ls_number_restraints     175
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0502
_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^)+(0.1018P)^2^+15.2100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1483
_refine_ls_wR_factor_ref         0.1520
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3772
_reflns_number_total             4275
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c01844_si_004.cif
_cod_data_source_block           p6mmm_a
_cod_depositor_comments
'Adding full bibliography for 4517880--4517884.cif.'
_cod_original_cell_volume        22246.7(8)
_cod_database_code               4517880
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.860
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 Zr1_$1-O2_$2
 2.19 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Ni2 \\sim Ni1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(O4A) = Uanis(O4)
Uanis(O3) = Uanis(O3A)
Uanis(Ni2) = Uanis(Ni1)
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: O3(0.25) Ni2(0.05) O4A(0.375) O4(0.125) O3A(0.5) Ni1(0.06)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C11(H11), C4(H4), C9(H9), C7(H7), C6(H6)
;
_olex2_submission_special_instructions 'No special instructions were received'