X-ray Crystallography and Magnetic Studies of a Stable Macrocyclic Tetranitroxide. Intramolecular Dimer of Nitroxides in a Constrained Geometry of the Upper Rim of Calix[4]arene
Andrzej Rajca; Maren Pink; Teerapat Rojsajjakul; Kan Lu; Hua Wang; Suchada Rajca; Journal of the American Chemical Society 125 (2003) 8534–8538; doi:10.1021/ja034115p

data_4113890
_publ_contact_author_address
;
        Department of Chemistry 
        University of Nebraska, Lincoln, NE 68588-0304.
        USA
;
_publ_contact_author_email       arajca1@unl.edu
_publ_contact_author_name        'Rajca, Andrzej'
_publ_section_title
;
 X-ray Crystallography and Magnetic Studies of a Stable Macrocyclic
 Tetranitroxide. Intramolecular Dimer of Nitroxides in a Constrained
 Geometry of the Upper Rim of Calix[4]arene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8534
_journal_page_last               8538
_journal_paper_doi               10.1021/ja034115p
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         'C88 H112 N4 O8, 2 (C H4 O)'
_chemical_formula_sum            'C90 H120 N4 O10'
_chemical_formula_weight         1417.90
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_method           SHELXL-97
_cell_angle_alpha                95.487(9)
_cell_angle_beta                 90.497(15)
_cell_angle_gamma                100.881(15)
_cell_formula_units_Z            2
_cell_length_a                   10.260(2)
_cell_length_b                   13.106(4)
_cell_length_c                   32.814(11)
_cell_measurement_reflns_used    935
_cell_measurement_temperature    95(2)
_cell_measurement_theta_max      19.34
_cell_measurement_theta_min      2.23
_cell_volume                     4312(2)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'KAPPASMART, Prototype, ChemMatCARS, APS'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_publication_material  'SHELXTL, Bruker'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al. 1992)'
_diffrn_ambient_temperature      95(2)
_diffrn_measured_fraction_theta_full 0.890
_diffrn_measured_fraction_theta_max 0.890
_diffrn_measurement_device_type  'Kappa geometry Bruker, 2x2 1K CCDs'
_diffrn_measurement_method       phi-scans
_diffrn_radiation_monochromator  'two Diamond 111'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_wavelength     0.55942
_diffrn_reflns_av_R_equivalents  0.1037
_diffrn_reflns_av_sigmaI/netI    0.1218
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            27185
_diffrn_reflns_theta_full        19.63
_diffrn_reflns_theta_max         19.63
_diffrn_reflns_theta_min         0.98
_exptl_absorpt_coefficient_mu    0.045
_exptl_absorpt_correction_T_max  0.9998
_exptl_absorpt_correction_T_min  0.9977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing (1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.092
_exptl_crystal_description       needle
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1071
_refine_ls_number_reflns         13938
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.1655
_refine_ls_R_factor_gt           0.1253
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1242P)^2^+15.8047P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3164
_refine_ls_wR_factor_ref         0.3361
_reflns_number_gt                8916
_reflns_number_total             13938
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja034115psi20030110_103755_1.cif
_cod_data_source_block           umnaps5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multi-scans' was replaced
with the value 'multi-scan' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_cell_volume        4311(2)
_cod_database_code               4113890