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_4132235
_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 N6 Se K O3, C2 H4 O0.5'
_chemical_formula_sum            'C59 H91 Cu3 K N6 O3.5 Se'
_chemical_formula_weight         1249.05
_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-2014/6
_audit_update_record
; 
2016-04-28 # Formatted by publCIF 
  
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.631(2)
_cell_length_b                   13.8788(13)
_cell_length_c                   18.5349(18)
_cell_measurement_reflns_used    3248
_cell_measurement_temperature    230(2)
_cell_measurement_theta_max      20.92
_cell_measurement_theta_min      2.26
_cell_volume                     6078.9(10)
_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-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      230(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1535
_diffrn_reflns_av_unetI/netI     0.1398
_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       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            59342
_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         27.500
_diffrn_reflns_theta_min         1.702
_exptl_absorpt_coefficient_mu    1.755
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6258
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2620
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.070
_refine_diff_density_max         1.057
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.117
_refine_ls_abs_structure_details
; 
 Flack x determined using 2833 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.018(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     741
_refine_ls_number_reflns         13953
_refine_ls_number_restraints     386
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.1421
_refine_ls_R_factor_gt           0.0618
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0729P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1324
_refine_ls_wR_factor_ref         0.1652
_reflns_Friedel_coverage         0.940
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                7819
_reflns_number_total             13953
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b02508_si_003.cif
_cod_data_source_block           GD140
_cod_original_formula_sum        'C59 H91 Cu3 K N6 O3.50 Se'
_cod_database_code               4132235
_shelx_estimated_absorpt_t_min   0.732
_shelx_estimated_absorpt_t_max   0.887
_shelxl_version_number           2014/6
_shelx_res_checksum              91777
_shelx_hkl_checksum              29407