Electronic Structural Analysis of Copper(II)-TEMPO/ABNO Complexes Provides Evidence for Copper(I)-Oxoammonium Character.
Walroth, Richard C.; Miles, Kelsey C.; Lukens, James T.; MacMillan, Samantha N.; Stahl, Shannon S.; Lancaster, Kyle M.; Journal of the American Chemical Society 139 (2017) 13507–13517; doi:10.1021/jacs.7b07186

data_4131590
_publ_section_title
;
 Electronic Structural Analysis of Copper(II)-TEMPO/ABNO Complexes
 Provides Evidence for Copper(I)-Oxoammonium Character.
;
_journal_issue                   38
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13507
_journal_page_last               13517
_journal_paper_doi               10.1021/jacs.7b07186
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C16 H28 Br4 Cu2 N2 O2'
_chemical_formula_sum            'C16 H28 Br4 Cu2 N2 O2'
_chemical_formula_weight         727.12
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-12-04
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.35(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.8100(14)
_cell_length_b                   13.680(3)
_cell_length_c                   11.660(2)
_cell_measurement_reflns_used    5018
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.239
_cell_measurement_theta_min      4.982
_cell_volume                     1086.2(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2130
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.169
_diffrn_reflns_theta_min         2.295
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.329
_exptl_absorpt_correction_T_max  0.190123
_exptl_absorpt_correction_T_min  0.064486
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
TWINABS was used for absorption correction. 3727 Corrected reflections written to file twin5a.hkl
 Reflections merged according to point-group 2/m   
 Single reflections that also occur in composites omitted
 Minimum and maximum apparent transmission:  0.064486  0.190123
 Additional spherical absorption correction applied with mu*r =  1.8000
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    2.223
_exptl_crystal_description       block
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.179
_refine_diff_density_min         -1.077
_refine_diff_density_rms         0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.196
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         2130
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.195
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0731P)^2^+1.0991P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1098
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2124
_reflns_number_total             2130
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b07186_si_002.cif
_cod_data_source_block           stahl204
_cod_database_code               4131590
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5 0.5
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Restrained distances
 C7-C4 \\sim C7-C6 \\sim C8-C6 \\sim C8-C1 \\sim C4-C2 \\sim C5-C2 \\sim C5-C3
\\sim C3-C1
 with sigma of 0.005
4.a Ternary CH refined with riding coordinates:
 C1(H1), C4(H4)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2a,H2b), C3(H3a,H3b), C5(H5a,H5b), C6(H6a,H6b), C7(H7a,H7b), C8(H8a,H8b)
;
_shelx_res_checksum              19052
_shelx_hkl_checksum              96382
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'