Studies of the Pathways Open to Copper Water Oxidation Catalysts Containing Proximal Hydroxy Groups During Basic Electrocatalysis.
Gerlach, Deidra L.; Bhagan, Salome; Cruce, Alex A.; Burks, Dalton B.; Nieto, Ismael; Truong, Hai T.; Kelley, Steven P.; Herbst-Gervasoni, Corey J; Jernigan, Katherine L.; Bowman, Michael K.; Pan, Shanlin; Zeller, Matthias; Papish, Elizabeth T.; Inorganic chemistry  (2014) 141203162841007–; doi:10.1021/ic501018a

data_4341771
_publ_section_title
;
 Studies of the Pathways Open to Copper Water Oxidation Catalysts
 Containing Proximal Hydroxy Groups During Basic Electrocatalysis.
;
_journal_name_full               'Inorganic chemistry'
_journal_page_first              141203162841007
_journal_paper_doi               10.1021/ic501018a
_journal_year                    2014
_chemical_formula_moiety         '2(C24 H24 Cu N5 O7), Cu N4 O12'
_chemical_formula_sum            'C48 H48 Cu3 N14 O26'
_chemical_formula_weight         1427.62
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                67.278(5)
_cell_angle_beta                 74.688(5)
_cell_angle_gamma                77.286(5)
_cell_formula_units_Z            1
_cell_length_a                   10.800(4)
_cell_length_b                   11.765(4)
_cell_length_c                   12.475(5)
_cell_measurement_reflns_used    4526
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.1392
_cell_measurement_theta_min      2.3948
_cell_volume                     1397.7(9)
_computing_cell_refinement       'SAINT V8.18C (Bruker, 2012)'
_computing_data_collection       'Apex2 v2012.4-3 (Bruker, 2012)'
_computing_data_reduction        'SAINT V8.18C (Bruker, 2012)'
_computing_molecular_graphics    'Shelxtl (Bruker, 2003)'
_computing_publication_material  'Shelxtl (Bruker, 2003)'
_computing_structure_refinement
;  
SHELXL-2013 (Sheldrick, 2013), 
SHELXLE Rev609 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Bruker AXS SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            31697
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.665
_diffrn_reflns_theta_min         2.112
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    1.233
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6350
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 v2012.4-3 (Bruker, 2012)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_description       block
_exptl_crystal_F_000             729
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.626
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         8221
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0412P)^2^+0.7602P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0897
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6460
_reflns_number_total             8221
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic501018a_si_002.cif
_cod_data_source_block           complex3_CJHG100_13mz070_0m
_cod_original_cell_volume        1397.8(9)
_cod_database_code               4341771
_shelx_estimated_absorpt_t_min   0.799
_shelx_estimated_absorpt_t_max   0.887
_shelxl_version_number           2012-9
_shelx_res_checksum              27523
_shelx_hkl_checksum              41264