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_7116490
_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_moiety         'C22 H24 Cr N5 O2, 0.5(C4 H8 O2), 2(Cl O4)'
_chemical_formula_sum            'C24 H28 Cl2 Cr N5 O11'
_chemical_formula_weight         685.41
_chemical_name_common            1
_chemical_name_systematic
'N,N,N-tris(2-pyridylmethyl)ethylenediamine-N-acetate-chromium(III) diperchlorate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2014-10-29 deposited with the CCDC.
2015-01-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.647(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.3004(14)
_cell_length_b                   12.4635(11)
_cell_length_c                   13.5694(12)
_cell_measurement_reflns_used    9278
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.63
_cell_measurement_theta_min      2.53
_cell_volume                     2755.6(4)
_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., 2006) and POV-RAY (Cason, 2003)'
_computing_publication_material  'SHELX-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 9.1
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_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  0.0321
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            88931
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.706
_diffrn_reflns_theta_min         2.057
_diffrn_source                   'fine-focus sealed-tube'
_exptl_absorpt_coefficient_mu    0.680
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1 (Sheldrick, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_description       block
_exptl_crystal_F_000             1412
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         8510
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0457P)^2^+1.5468P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0878
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7533
_reflns_number_total             8510
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc08785b2.cif
_cod_data_source_block           publication_text
_cod_database_code               7116490
_chemical_name_id                '[Cr(tpena)](ClO4)2(C4H8O2)0.5'
_shelx_estimated_absorpt_t_min   0.727
_shelx_estimated_absorpt_t_max   0.876
_shelxl_version_number           2013-4
_shelx_res_checksum              92568