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_4516742
_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 H360 Cu18 N48 O90)'
_chemical_formula_sum            'C78 H60 Cu3 N8 O15'
_chemical_formula_weight         1539.96
_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             2018-06-26
_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                   15.598(7)
_cell_length_b                   15.598(7)
_cell_length_c                   59.01(2)
_cell_measurement_reflns_used    9889
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.90
_cell_measurement_theta_min      2.29
_cell_volume                     12434(9)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0301
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       77
_diffrn_reflns_limit_l_min       -77
_diffrn_reflns_number            44916
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.875
_diffrn_reflns_theta_min         2.044
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.826
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6525
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0586 before and 0.0448 after correction. The Ratio of minimum to maximum transmission is 0.8749. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       cube
_exptl_crystal_F_000             4746
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.31
_platon_squeeze_details
;
TITL mo_lan1_0m_a.res in R-3
CELL   15.5980   15.5980   59.0100     90.00     90.00    120.00
SPGR R-3
C101 0.296 0.468 0.164 !       6.62 eA-3
C102 0.337 0.675 0.102 !       2.05 eA-3
Q103 0.544 0.996 0.505 !       1.60 eA-3
Q104 0.845 0.155 0.418 !       1.59 eA-3
C105 1.001 0.999 0.457 !       1.47 eA-3
C106 0.998 0.986 0.000 !       1.38 eA-3
C107 1.001 1.003 0.652 !       1.37 eA-3
C108 0.095 1.001 0.434 !       1.28 eA-3
C109 0.736 0.501 0.327 !       1.21 eA-3
C110 0.705 0.234 0.328 !       1.07 eA-3
Q111 0.158 0.596 0.243 !       0.87 eA-3
Q112 0.057 0.765 0.856 !       0.82 eA-3
C113 0.998 0.997 0.590 !       0.80 eA-3
C114 0.389 0.741 0.304 !       0.80 eA-3
Q115 0.704 0.766 0.534 !       0.78 eA-3
C116 0.478 0.689 0.087 !       0.66 eA-3
Q117 0.265 0.197 0.891 !       0.65 eA-3
C118 0.649 0.326 0.937 !       0.62 eA-3
Q119 0.280 0.223 0.882 !       0.60 eA-3
C120 0.287 0.654 0.289 !       0.60 eA-3
C121 0.629 0.326 0.956 !       0.59 eA-3
Q122 0.080 0.377 0.070 !       0.53 eA-3
Q123 0.095 0.092 0.288 !       0.53 eA-3
Q124 0.514 0.437 0.254 !       0.52 eA-3
Q125 0.999 0.994 0.297 !       0.50 eA-3
;
_refine_diff_density_max         1.303
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         6590
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0498
_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^)+(0.0708P)^2^+33.1916P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1354
_refine_ls_wR_factor_ref         0.1413
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5598
_reflns_number_total             6590
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b04887_si_004.cif
_cod_data_source_block           mo_lan1_0m_sq
_cod_original_cell_volume        12433(12)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4516742
_shelx_shelxl_version_number     2014/7
_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)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11),
 C12(H12), C15(H15), C16(H16), C18(H18), C19(H19), C22(H22), C23(H23), C25(H25),
  C26(H26)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'