Nitroxide-nitroxide and nitroxide-metal distance measurements in transition metal complexes with two or three paramagnetic centres give access to thermodynamic and kinetic stabilities.
Giannoulis, A.; Ackermann, K.; Spindler, P. E.; Higgins, C.; Cordes, D. B.; Slawin, A. M. Z.; Prisner, T. F.; Bode, B. E.; Physical chemistry chemical physics : PCCP 20 (2018) 11196–11205; doi:10.1039/c8cp01611a

data_7230392
_publ_section_title
;
 Nitroxide-nitroxide and nitroxide-metal distance measurements in
 transition metal complexes with two or three paramagnetic centres give
 access to thermodynamic and kinetic stabilities.
;
_journal_issue                   16
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              11196
_journal_page_last               11205
_journal_paper_doi               10.1039/c8cp01611a
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C15 H17 I N O3'
_chemical_formula_sum            'C15 H17 I N O3'
_chemical_formula_weight         386.21
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-04-13
_audit_creation_method           'by CrystalStructure 4.1'
_audit_update_record
;
2016-08-04 deposited with the CCDC.
2018-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                105.821(3)
_cell_angle_beta                 94.648(3)
_cell_angle_gamma                105.915(4)
_cell_formula_units_Z            2
_cell_length_a                   9.0407(16)
_cell_length_b                   9.359(2)
_cell_length_c                   10.1910(19)
_cell_measurement_reflns_used    2685
_cell_measurement_temperature    173
_cell_measurement_theta_max      25.40
_cell_measurement_theta_min      2.40
_cell_volume                     786.4(3)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b32'
_computing_data_collection
'CrystalClear-SM Expert 2.1 b32 (Rigaku, 2014)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b32'
_computing_molecular_graphics    'CrystalStructure 4.1'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF99-PATTY (Gould, et al., 1999)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 11.628
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.990
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_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9770
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.406
_diffrn_reflns_theta_min         2.107
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.043
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_correction_T_min  0.548
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_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             382.00
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dichloromethane/hexane'
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
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_refine_diff_density_min         -0.29
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_reflns         2873
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0234
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0249P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0551
_refine_ls_wR_factor_ref         0.0563
_reflns_number_gt                2630
_reflns_number_total             2873
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
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_cod_depositor_comments
'Adding full bibliography for 7230391--7230392.cif.'
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