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_4516743
_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         '0.17(C468 H396 Co18 N48 O108)'
_chemical_formula_sum            'C78 H66 Co3 N8 O18'
_chemical_formula_weight         1580.17
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-30
_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                   15.7439(10)
_cell_length_b                   15.7439(10)
_cell_length_c                   61.146(4)
_cell_measurement_reflns_used    9953
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.71
_cell_measurement_theta_min      2.24
_cell_volume                     13125.7(15)
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0216
_diffrn_reflns_av_unetI/netI     0.0156
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       79
_diffrn_reflns_limit_l_min       -70
_diffrn_reflns_number            42159
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         0.999
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.627
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0386 before and 0.0342 after correction. The Ratio of minimum to maximum transmission is 0.9316. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_description       block
_exptl_crystal_F_000             4890
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.34
_platon_squeeze_details
;
TITL mo_tca-co_0m_a.res in R-3
CELL   15.7439   15.7439   61.1460     90.00     90.00    120.00
SPGR R-3
C101 0.530 0.706 0.163 !       6.09 eA-3
C102 0.580 0.427 0.340 !       4.77 eA-3
C103 1.001 0.995 0.367 !       2.64 eA-3
C104 1.000 0.992 0.391 !       2.03 eA-3
C105 0.027 0.953 0.400 !       1.26 eA-3
C106 0.423 0.644 0.306 !       1.24 eA-3
C107 0.340 0.669 0.320 !       1.15 eA-3
Q108 0.916 0.170 0.562 !       1.12 eA-3
C109 0.055 0.852 0.453 !       0.95 eA-3
C110 0.340 0.670 0.211 !       0.88 eA-3
C111 0.755 0.421 0.708 !       0.83 eA-3
Q112 0.390 0.420 0.203 !       0.74 eA-3
Q113 0.188 0.659 0.601 !       0.60 eA-3
C114 0.060 0.083 0.454 !       0.57 eA-3
Q115 0.723 0.923 0.125 !       0.51 eA-3
Q116 0.215 0.466 0.102 !       0.51 eA-3
;
_refine_diff_density_max         1.096
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         6663
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0407
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0748P)^2^+20.1104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1224
_refine_ls_wR_factor_ref         0.1299
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5747
_reflns_number_total             6663
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b04887_si_003.cif
_cod_data_source_block           mo_tca-co_0m_sq
_cod_original_cell_volume        13125.7(19)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4516743
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.815
_shelx_estimated_absorpt_t_min   0.779
_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.a Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C6(H6), C4(H4), C25(H25), C26(H26), C22(H22), C23(H23),
 C11(H11), C14(H14), C8(H8), C19(H19), C17(H17), C15(H15), C18(H18), C9(H9),
 C13(H13), C12(H12)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'