Formation of a Mixed-Valence Cu(I)/Cu(II) Metal-Organic Framework with the Full Light Spectrum and High Selectivity of CO2 Photoreduction into CH4
Gao, Yajun; Bai, Junfeng; Zhang, Lei; Gu, Yuming; Zhang, Wen-Wei; Pan, Yi; Fang, Wei-hai; Ma, Jing; Lan, Ya-Qian; Chemical Science  (2020) –; doi:10.1039/D0SC03754K

data_1558961
_publ_section_title
;
 Formation of a Mixed-Valence Cu(I)/Cu(II) Metal-Organic Framework with
 the Full Light Spectrum and High Selectivity of CO2 Photoreduction into
 CH4
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC03754K
_journal_year                    2020
_chemical_formula_moiety         'C33 H45 Cu13 I11 N12 O7'
_chemical_formula_sum            'C33 H45 Cu13 I11 N12 O7'
_chemical_formula_weight         2943.86
_chemical_name_systematic        NJU-Bai61
_space_group_crystal_system      cubic
_space_group_IT_number           217
_space_group_name_Hall           'I -4 2 3'
_space_group_name_H-M_alt        'I -4 3 m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-10-11 deposited with the CCDC.	2020-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.1585(14)
_cell_length_b                   25.1585(14)
_cell_length_c                   25.1585(14)
_cell_measurement_reflns_used    4494
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      20.65
_cell_measurement_theta_min      2.28
_cell_volume                     15924.1(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1345
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            59047
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.012
_diffrn_reflns_theta_max         25.012
_diffrn_reflns_theta_min         1.983
_exptl_absorpt_coefficient_mu    7.699
_exptl_absorpt_correction_T_max  0.168
_exptl_absorpt_correction_T_min  0.146
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.456
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             10744
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_platon_squeeze_details
;
;
_refine_diff_density_max         3.449
_refine_diff_density_min         -3.014
_refine_diff_density_rms         0.386
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.03(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.184
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         2593
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.181
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0649
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1155P)^2^+402.1500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1819
_refine_ls_wR_factor_ref         0.1992
_reflns_Friedel_coverage         0.863
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2374
_reflns_number_total             2593
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc03754k2.cif
_cod_data_source_block           S_a
_cod_original_cell_volume        15924(3)
_cod_database_code               1558961
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.578
_shelx_estimated_absorpt_t_max   0.578
_shelx_res_checksum              83875