Autocatalytic O2 Cleavage by an OCO3-Trianionic Pincer CrIII Complex: Isolation and Characterization of the Autocatalytic Intermediate [CrIV]2(μ-O) Dimer
Matthew E. O'Reilly; Trevor J. Del Castillo; Joseph M. Falkowski; Vasanth Ramachandran; Mekhala Pati; Marie C. Correia; Khalil A. Abboud; Naresh S. Dalal; David E. Richardson; Adam S. Veige; Journal of the American Chemical Society 133 (2011) 13661–13673; doi:10.1021/ja2050474

data_4106666
_publ_section_title
;
 Autocatalytic O2 Cleavage by an OCO3-Trianionic Pincer CrIII Complex:
 Isolation and Characterization of the Autocatalytic Intermediate
 [CrIV]2(\m-O) Dimer
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13661
_journal_page_last               13673
_journal_paper_doi               10.1021/ja2050474
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C68 H90 Cr2 O9'
_chemical_formula_weight         1155.40
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2008-03-18 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 104.655(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.7961(16)
_cell_length_b                   11.9905(8)
_cell_length_c                   21.8533(14)
_cell_measurement_reflns_used    92
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     6286.0(7)
_computing_cell_refinement
'Bruker SMART v5.624 & SAINT 6.36a (Bruker 1998)'
_computing_data_collection       'Bruker SMART v5.624 (Bruker 1998)'
_computing_data_reduction        'Bruker SHELXTL v6.14 (Bruker 2000)'
_computing_molecular_graphics    'Bruker SHELXTL v6.14'
_computing_publication_material  'Bruker SHELXTL v6.14'
_computing_structure_refinement  'Bruker SHELXTL v6.14'
_computing_structure_solution    'Bruker SHELXTL v6.14'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'SMART CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_sigmaI/netI    0.0678
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20039
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.70
_diffrn_standards_decay_%        1
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.400
_exptl_absorpt_correction_T_max  0.9461
_exptl_absorpt_correction_T_min  0.9136
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
'based on measured indexed crystal faces, Bruker SHELXTL  v6.12 (Bruker 1998)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2472
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         7215
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0518
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0719P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1227
_refine_ls_wR_factor_ref         0.1345
_reflns_number_gt                5027
_reflns_number_total             7215
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja2050474_si_001.cif
_cod_data_source_block           jf07
_cod_database_code               4106666