Monometallic Catalytic Models Hosted in Stable Metal‒Organic Frameworks for Tunable CO2 Photoreduction
Wang, Xiao-Kun; Liu, Jiang; Zhang, Lei; Dong, Long-Zhang; Li, Shun-Li; Kan, Yu-He; Li, Dong-Sheng; Lan, Ya-Qian; ACS Catalysis 9 (2019) 1726–; doi:10.1021/acscatal.8b04887

data_4516744
_publ_section_title
;
 Monometallic Catalytic Models Hosted in Stable Metal--Organic Frameworks
 for Tunable CO2 Photoreduction
;
_journal_issue                   3
_journal_name_full               'ACS Catalysis'
_journal_page_first              1726
_journal_paper_doi               10.1021/acscatal.8b04887
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C468 H396 N48 Ni18 O108, 27(H2 O)'
_chemical_formula_sum            'C468 H450 N48 Ni18 O135'
_chemical_formula_weight         9963.51
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-11-13
_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            1
_cell_length_a                   15.7128(10)
_cell_length_b                   15.7128(10)
_cell_length_c                   60.539(4)
_cell_measurement_reflns_used    9959
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.25
_cell_volume                     12944.1(14)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       78
_diffrn_reflns_limit_l_min       -78
_diffrn_reflns_number            42225
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.870
_diffrn_reflns_theta_min         1.641
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.720
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6435
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0458 before and 0.0344 after correction. The Ratio of minimum to maximum transmission is 0.8629. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             5178
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_platon_squeeze_details
;
TITL mo_tca_ni_0m_a.res in R-3
CELL   15.7128   15.7128   60.5390     90.00     90.00    120.00
SPGR R-3
C101 0.332 0.675 0.300 !       1.95 eA-3
C102 1.000 1.008 0.344 !       1.34 eA-3
C103 1.000 1.006 0.609 !       1.26 eA-3
Q104 0.750 0.922 0.436 !       1.18 eA-3
Q105 0.796 0.457 0.341 !       1.14 eA-3
C106 0.252 0.686 0.054 !       1.08 eA-3
C107 0.107 0.984 0.635 !       1.04 eA-3
Q108 0.080 0.988 0.609 !       1.03 eA-3
Q109 0.531 0.719 0.215 !       0.90 eA-3
Q110 0.939 0.919 0.396 !       0.90 eA-3
C111 0.656 0.399 0.935 !       0.79 eA-3
Q112 0.472 0.895 0.094 !       0.76 eA-3
C113 1.002 1.005 0.453 !       0.68 eA-3
Q114 0.875 0.018 0.423 !       0.62 eA-3
Q115 0.387 0.655 0.224 !       0.58 eA-3
Q116 0.763 0.517 0.320 !       0.58 eA-3
Q117 0.309 0.141 0.415 !       0.50 eA-3
;
_refine_diff_density_max         1.211
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         6792
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0886P)^2^+27.5483P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1422
_refine_ls_wR_factor_ref         0.1511
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5615
_reflns_number_total             6792
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b04887_si_002.cif
_cod_data_source_block           mo_tca_ni_0m_sq
_cod_original_cell_volume        12944.1(18)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4516744
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.858
_shelx_estimated_absorpt_t_min   0.840
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: O3W(0.5) H3WA(0.5) H3WB(0.5)
3.a Riding coordinates:
 O3W(H3WA,H3WB)
3.b Free rotating group:
 O4W(H4WA,H4WB)
3.c Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
3.d Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), C7(H7), C11(H11), C10(H10), C6(H6), C26(H26), C14(H14),
 C13(H13), C19(H19), C20(H20), C25(H25), C24(H24), C18(H18), C15(H15), C16(H16),
  C22(H22), C21(H21)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'