Hydroxo-Bridged Dicopper(II,III) and -(III,III) Complexes: Models for Putative Intermediates in Oxidation Catalysis.
Halvagar, Mohammad Reza; Solntsev, Pavlo V.; Lim, Hyeongtaek; Hedman, Britt; Hodgson, Keith O.; Solomon, Edward I.; Cramer, Christopher J.; Tolman, William B.; Journal of the American Chemical Society 136 (2014) 7269–7272; doi:10.1021/ja503629r

data_4121798
_publ_section_title
;
 Hydroxo-Bridged Dicopper(II,III) and -(III,III) Complexes: Models for
 Putative Intermediates in Oxidation Catalysis.
;
_journal_issue                   20
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7269
_journal_page_last               7272
_journal_paper_doi               10.1021/ja503629r
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety
'C52 H28 Cu4 N12 O9, 2(C3 H7 N O), 2(C4 H12 N), 4(H2O)'
_chemical_formula_sum            'C66 H74 Cu4 N16 O15'
_chemical_formula_weight         1585.57
_chemical_name_common            '[NMe_4]_2 [L_2 Cu_4 (\m_4-O)]'
_chemical_name_systematic        ?
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.690(2)
_cell_length_b                   17.558(2)
_cell_length_c                   24.517(3)
_cell_measurement_reflns_used    1904
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.72
_cell_measurement_theta_min      2.32
_cell_volume                     7184.5(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruke APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97   (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1892
_diffrn_reflns_av_unetI/netI     0.2026
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            54128
_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         26.000
_diffrn_reflns_theta_min         1.661
_exptl_absorpt_coefficient_mu    1.243
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6527
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_description       block
_exptl_crystal_F_000             3272
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.434
_refine_diff_density_min         -0.991
_refine_diff_density_rms         0.160
_refine_ls_abs_structure_details
;
 Flack x determined using 2195 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.080(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     899
_refine_ls_number_reflns         14128
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.1846
_refine_ls_R_factor_gt           0.0917
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1293P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2086
_refine_ls_wR_factor_ref         0.2587
_reflns_Friedel_coverage         0.830
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                7314
_reflns_number_total             14128
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja503629r_si_001.cif
_cod_data_source_block           Comp1
_cod_depositor_comments
'Adding full bibliography for 4121798--4121800.cif.'
_cod_database_code               4121798
_shelx_estimated_absorpt_t_min   0.755
_shelx_estimated_absorpt_t_max   0.886
_shelxl_version_number           2013-4
_shelx_res_checksum              72438
_shelx_hkl_checksum              53055