Spectroscopic capture and reactivity of S = 1/2 nickel(III)-oxygen intermediates in the reaction of a NiII-salt with mCPBA
Florian Felix Pfaff; Florian Heims; Subrata Kundu; Stefan Mebs; Kallol Ray; Chem.Commun. 48 (2012) 3730–; doi:10.1039/c2cc30716b

data_7107536
_publ_section_title
;
 Spectroscopic capture and reactivity of S = 1/2 nickel(III)-oxygen
 intermediates in the reaction of a NiII-salt with mCPBA
;
_journal_name_full               Chem.Commun.
_journal_page_first              3730
_journal_paper_doi               10.1039/c2cc30716b
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C22 H48 F3 N10 Ni O3 S, C F3 O3 S'
_chemical_formula_sum            'C23 H48 F6 N10 Ni O6 S2'
_chemical_formula_weight         797.54
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.4410(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.9694(2)
_cell_length_b                   15.6473(3)
_cell_length_c                   18.9697(3)
_cell_measurement_reflns_used    100643
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.61
_cell_measurement_theta_min      2.15
_cell_volume                     3530.39(11)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      ' 360 frames, detector distance = 100 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0709
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            68675
_diffrn_reflns_theta_full        29.50
_diffrn_reflns_theta_max         29.50
_diffrn_reflns_theta_min         2.12
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           45
_diffrn_source_power             2.25
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.751
_exptl_absorpt_correction_T_max  0.8071
_exptl_absorpt_correction_T_min  0.6129
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'STOE X-RED'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_description       block
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.570
_exptl_crystal_size_mid          0.433
_exptl_crystal_size_min          0.360
_refine_diff_density_max         1.049
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.122
_refine_ls_extinction_coef       0.0131(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.277
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     519
_refine_ls_number_reflns         9842
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      1.309
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0601
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0475P)^2^+10.0540P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1655
_refine_ls_wR_factor_ref         0.1677
_reflns_d_resolution_high        0.722
_reflns_d_resolution_low         9.585
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                8690
_reflns_number_total             9845
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc30716b.txt
_cod_data_source_block           c:fpp13
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7107536