Electrocatalytic Water Oxidation by a Homogeneous Copper Catalyst Disfavors Single-Site Mechanisms.
Koepke, Sara J.; Light, Kenneth M.; VanNatta, Peter E.; Wiley, Keaton M.; Kieber-Emmons, Matthew T; Journal of the American Chemical Society 139 (2017) 8586–8600; doi:10.1021/jacs.7b03278

data_4126224
_publ_section_title
;
 Electrocatalytic Water Oxidation by a Homogeneous Copper Catalyst
 Disfavors Single-Site Mechanisms.
;
_journal_issue                   25
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8586
_journal_page_last               8600
_journal_paper_doi               10.1021/jacs.7b03278
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety
'C40 H46 N8 O2 Cu2, 2(C F3 O3 S), 0.5(C4 H10 O)'
_chemical_formula_sum            'C44 H51 Cu2 F6 N8 O8.5 S2'
_chemical_formula_weight         1133.12
_chemical_name_common            mke005
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.5045(8)
_cell_length_b                   32.977(2)
_cell_length_c                   20.6961(11)
_cell_measurement_reflns_used    9076
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.8571
_cell_measurement_theta_min      2.3247
_cell_volume                     9899.3(10)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection
'Bruker Instrument Service 2014.9.0.0 (Bruker AXS Inc.)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics
'ORTEP-3 (L. J. Farrugia, J. Appl. Cryst. (2012),45, 849-854.)'
_computing_publication_material  'APEX2 v2014.9-0 (Bruker AXS Inc.)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/9 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEX II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            83792
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         1.85
_diffrn_source                   'fine-focus tube'
_diffrn_source_type              'Siemans KFFMO2K-90'
_exptl_absorpt_coefficient_mu    1.027
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G. M. (2014). SADABS V2014/4 BRUKER AXS Inc. Madison WI 53711 USA
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4664
_exptl_crystal_size_max          0.392
_exptl_crystal_size_mid          0.266
_exptl_crystal_size_min          0.140
_refine_diff_density_max         1.190
_refine_diff_density_min         -0.415
_refine_ls_abs_structure_details
;
Flack x determined using 903 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.332(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1271
_refine_ls_number_reflns         23433
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0544P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.0959
_reflns_number_gt                19990
_reflns_number_total             23433
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b03278_si_001.cif
_cod_data_source_block           I
_cod_depositor_comments
;
          Adding full bibliography for 4126224.cif.'

2020-05-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety
'2(C40 H46 N8 O2 Cu2), 4(C F3 O3 S), (C4 H10 O)'
_cod_original_formula_sum        'C88 H102 Cu4 F12 N16 O17 S4'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     2266.25
_cod_database_code               4126224
_shelx_res_checksum              62662
_shelx_hkl_checksum              84156