Conformationally Constrained, Stable, Triplet Ground State (S=1) Nitroxide Diradicals. Antiferromagnetic Chains of S=1 Diradicals
Andrzej Rajca; Masahiro Takahashi; Maren Pink; Gaëlle Spagnol; Suchada Rajca; Journal of the American Chemical Society 129 (2007) 10159–10170; doi:10.1021/ja0712017

data_4109781
_publ_section_title
;
 Conformationally Constrained, Stable, Triplet Ground State (S=1)
 Nitroxide Diradicals. Antiferromagnetic Chains of S=1 Diradicals
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10159
_journal_page_last               10170
_journal_paper_doi               10.1021/ja0712017
_journal_volume                  129
_journal_year                    2007
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C36 H52 N4 O8, 2 C H2 Cl2'
_chemical_formula_sum            'C38 H56 Cl4 N4 O8'
_chemical_formula_weight         838.67
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 131.3080(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.4534(11)
_cell_length_b                   12.5714(6)
_cell_length_c                   17.3570(8)
_cell_measurement_reflns_used    8391
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      26.4
_cell_measurement_theta_min      2.3
_cell_volume                     4172.0(3)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2003), XTEL (loc. libr.)'
_computing_publication_material  'SHELXTL (Bruker, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
'0.30 degree frames measured for 15 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0345
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29506
_diffrn_reflns_theta_full        26.42
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         1.56
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_time  606
_diffrn_standards_number         142
_exptl_absorpt_coefficient_mu    0.338
_exptl_absorpt_correction_T_max  0.9511
_exptl_absorpt_correction_T_min  0.9264
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing; 1995'
_exptl_crystal_colour            'light brown'
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.248
_refine_diff_density_min         -1.431
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         8583
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0570
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1092P)^2^+6.8293P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1617
_refine_ls_wR_factor_ref         0.1699
_reflns_number_gt                7901
_reflns_number_total             8583
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0712017si20070219_032046.cif
_cod_data_source_block           06468
_cod_database_code               4109781