Countercations and Solvent Influence CO<sub>2</sub> Reduction to Oxalate by Chalcogen-Bridged Tricopper Cyclophanates.
Cook, Brian J.; Di Francesco, Gianna N.; Abboud, Khalil A.; Murray, Leslie J.; Journal of the American Chemical Society 140 (2018) 5696–5700; doi:10.1021/jacs.8b02508

data_4132236
_publ_section_title
;
 Countercations and Solvent Influence CO<sub>2</sub> Reduction to Oxalate
 by Chalcogen-Bridged Tricopper Cyclophanates.
;
_journal_issue                   17
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5696
_journal_page_last               5700
_journal_paper_doi               10.1021/jacs.8b02508
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C57 H87 Cu3 K N6 O3 S, C4 H8 O'
_chemical_formula_sum            'C61 H95 Cu3 K N6 O4 S'
_chemical_formula_weight         1238.20
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2014-07-08 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.4096(15)
_cell_length_b                   13.7260(9)
_cell_length_c                   18.4332(12)
_cell_measurement_reflns_used    9819
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     5923.0(7)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2 (Bruker, 2008)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2008)'
_computing_molecular_graphics    'SHELXL-2013 (Sheldrick, 2013)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II DUO'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            95608
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.496
_diffrn_reflns_theta_min         1.720
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.224
_exptl_absorpt_correction_T_max  0.9677
_exptl_absorpt_correction_T_min  0.8664
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'based on measured indexed crystal faces, Bruker SHELXTL  v6.14 (Bruker 2008)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_description       prisms
_exptl_crystal_F_000             2628
_exptl_crystal_size_max          0.226
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
; 
 Flack x determined using 5195 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   -0.014(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         13595
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0248
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0259P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0506
_refine_ls_wR_factor_ref         0.0522
_reflns_Friedel_coverage         0.939
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                11790
_reflns_number_total             13595
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b02508_si_002.cif
_cod_data_source_block           murr18
_cod_database_code               4132236
_shelx_estimated_absorpt_t_min   0.769
_shelx_estimated_absorpt_t_max   0.964
_shelxl_version_number           2013-3
_shelx_res_checksum              91242
_shelx_hkl_checksum              34195