The Gigantic {Ni<sub>36</sub>Gd<sub>102</sub>} Hexagon: A Sulfate-Templated "Star-of-David" for Photocatalytic CO<sub>2</sub> Reduction and Magnetic Cooling.
Chen, Wei-Peng; Liao, Pei-Qin; Jin, Peng-Bo; Zhang, Lei; Ling, Bo-Kai; Wang, Shi-Cheng; Chan, Yi-Tsu; Chen, Xiao-Ming; Zheng, Yan-Zhen; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.9b11543

data_4134234
_publ_section_title
;
 The Gigantic {Ni<sub>36</sub>Gd<sub>102</sub>} Hexagon: A
 Sulfate-Templated &quot;Star-of-David&quot; for Photocatalytic
 CO<sub>2</sub> Reduction and Magnetic Cooling.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b11543
_journal_year                    2020
_chemical_formula_sum            'C492 H1340 Br6 Gd102 N60 Ni36 O832 S54'
_chemical_formula_weight         41775.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 118.26(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   77.656(16)
_cell_length_b                   32.255(7)
_cell_length_c                   64.599(13)
_cell_measurement_reflns_used    59986
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.85
_cell_measurement_theta_min      1.892
_cell_volume                     142521(7)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       SADABS
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.8265
_diffrn_reflns_av_R_equivalents  0.114
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_number            129860
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        29.729
_diffrn_reflns_theta_max         29.848
_diffrn_reflns_theta_min         1.892
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    5.475
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.947
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       strip
_exptl_crystal_F_000             79912
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.050
_exptl_transmission_factor_max   0.761
_exptl_transmission_factor_min   0.581
_refine_diff_density_max         3.874
_refine_diff_density_min         -3.928
_refine_diff_density_rms         0.287
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     6057
_refine_ls_number_reflns         129860
_refine_ls_number_restraints     8254
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.2127
_refine_ls_R_factor_gt           0.1258
_refine_ls_shift/su_max          0.036
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0720P)^2^+10072.7305P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2789
_refine_ls_wR_factor_ref         0.3145
_reflns_Friedel_coverage         0.000
_reflns_number_gt                59986
_reflns_number_total             129860
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b11543_si_002.cif
_cod_data_source_block           Ni36Gd102
_cod_original_cell_volume        142518(61)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4134234
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.514
_shelx_estimated_absorpt_t_max   0.771
_platon_squeeze_void_probe_radius 1.20
_platon_ni36gd102_details
;
The 60 disordered methanol molecules, 130 disordered water molecules
and 6 NO3- anions per formula unit were removed by SQUEEZE.The values were 
calculated based on TG, elemental analysess and charge balance.
;
_shelx_res_checksum              88466
_shelx_hkl_checksum              78482