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_4517881
_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(C204 H96 Br12 Ni2.4 O103.8 Zr18)'
_chemical_formula_sum            'C34 H16 Br2 Ni0.4 O17.3 Zr3'
_chemical_formula_weight         1158.23
_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             2019-03-25
_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                   39.903(6)
_cell_length_b                   39.903(6)
_cell_length_c                   12.022(2)
_cell_measurement_reflns_used    9736
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      65.13
_cell_measurement_theta_min      2.56
_cell_volume                     16577(4)
_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      200.02
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.942
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            65061
_diffrn_reflns_point_group_measured_fraction_full 0.942
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.381
_diffrn_reflns_theta_min         1.278
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.429
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.6442
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0986 before and 0.0492 after correction. The Ratio of minimum to maximum transmission is 0.8560. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.696
_exptl_crystal_description       needle
_exptl_crystal_F_000             3358
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.474
_refine_diff_density_min         -1.547
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         5314
_refine_ls_number_restraints     161
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0567
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1259P)^2^+38.1740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1802
_refine_ls_wR_factor_ref         0.1869
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4878
_reflns_number_total             5314
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c01844_si_005.cif
_cod_data_source_block           xz121_0m_a
_cod_depositor_comments
'Adding full bibliography for 4517880--4517884.cif.'
_cod_original_cell_volume        16577(6)
_cod_original_formula_sum        'C34 H16 Br2 Ni0.40 O17.30 Zr3'
_cod_database_code               4517881
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.904
_shelx_estimated_absorpt_t_min   0.645
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 Ni1-O5
 2.1 with sigma of 0.02
 Ni2-O8
 2.39 with sigma of 0.001
3. 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
4. Others
 Fixed Sof: Ni2(0.05) Ni1(0.025) Ni3(0.025) O7(0.075) O9A(0.1) O9(0.15)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7)
;
_olex2_submission_special_instructions 'No special instructions were received'