Caught! Crystal trapping of a side-on peroxo bound to Cr(iv).
de Sousa, David P.; Bigelow, Jennifer O.; Sundberg, Jonas; Que, Lawrence; McKenzie, Christine J.; Chemical communications (Cambridge, England) 51 (2015) 2802–; doi:10.1039/c4cc08785b

data_7116489
_publ_section_title
;
 Caught! Crystal trapping of a side-on peroxo bound to Cr(iv).
;
_journal_issue                   14
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2802
_journal_paper_doi               10.1039/c4cc08785b
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C22 H33 Cl2 Cr N5 O19'
_chemical_formula_weight         794.42
_chemical_name_common            4
_chemical_name_systematic
'(N,N,N-tris(2-pyridylmethyl)ethylenediamine-N-acetate)chromium(IV)peroxo diperhlorate'
_chemical_properties_physical
'rapid decomposition though loss of co-crystallised molecules and possible auto oxidation'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2014-12-21 deposited with the CCDC.
2015-01-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 118.237(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2360(16)
_cell_length_b                   14.7664(16)
_cell_length_c                   16.0081(17)
_cell_measurement_temperature    150.0(2)
_cell_volume                     3172.9(6)
_computing_cell_refinement       'SAINT v.7.68a (Bruker, 2010)'
_computing_data_collection       'APEX2 v.2010.1-2 (Bruker Nonius, 2010)'
_computing_data_reduction        'SAINT v.7.68a (Bruker, 2010)'
_computing_molecular_graphics
'Mercury 3.11 (Macrae at al., 2008) and POV-RAY (Cason, 2004)'
_computing_publication_material  'SHELX-2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector_area_resol_mean 9.1
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker-Nonius X8APEX-II CCD'
_diffrn_measurement_method       'thin-slice \w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0816
_diffrn_reflns_av_unetI/netI     0.0607
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            43336
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.753
_diffrn_source                   'fine-focus sealed-tube'
_exptl_absorpt_coefficient_mu    0.623
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1 (Sheldrick, 2008)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_description       plate
_exptl_crystal_F_000             1647
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: 33% H2O2 in water'
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.040
_exptl_transmission_factor_max   0.7461
_exptl_transmission_factor_min   0.5698
_refine_diff_density_max         2.215
_refine_diff_density_min         -0.779
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     473
_refine_ls_number_reflns         6430
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1298
_refine_ls_R_factor_gt           0.1030
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1406P)^2^+33.1301P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_gt          0.2841
_refine_ls_wR_factor_ref         0.3020
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4722
_reflns_number_total             6430
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc08785b2.cif
_cod_data_source_block           publication_text
_cod_database_code               7116489
_chemical_name_id                '[CrO2(tpenaH)](ClO4)2(H2O2)4'
_shelx_estimated_absorpt_t_min   0.845
_shelx_estimated_absorpt_t_max   0.976
_shelxl_version_number           2014/6
_shelx_res_checksum              94904