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_4121800
_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'
_chemical_formula_sum            'C52 H28 Cu4 N12 O9'
_chemical_formula_weight         1219.02
_chemical_name_common            '[NMe_4]_2 [L_2 Cu_4 (\m_4-O)]'
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           121
_space_group_name_Hall           'I -4 2'
_space_group_name_H-M_alt        'I -4 2 m'
_symmetry_space_group_name_Hall  'I -4 2'
_symmetry_space_group_name_H-M   'I -4 2 m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.5216(7)
_cell_length_b                   14.5216(7)
_cell_length_c                   15.9314(11)
_cell_measurement_temperature    123(2)
_cell_volume                     3359.6(3)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13058
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.420
_diffrn_reflns_theta_min         4.119
_exptl_absorpt_coefficient_mu    1.868
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.5419
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.15(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         1637
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0684P)^2^+1.5902P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1052
_refine_ls_wR_factor_ref         0.1094
_reflns_Friedel_coverage         0.784
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1501
_reflns_number_total             1637
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja503629r_si_001.cif
_cod_data_source_block           Comp5
_cod_depositor_comments
'Adding full bibliography for 4121798--4121800.cif.'
_cod_original_cell_volume        3359.6(4)
_cod_database_code               4121800
_shelx_estimated_absorpt_t_min   0.767
_shelx_estimated_absorpt_t_max   0.807
_shelxl_version_number           2013-4
_shelx_res_checksum              73917
_shelx_hkl_checksum              99681
_shelx_fab_checksum              84028