A modular approach for the synthesis of nanometer-sized polynitroxide multi-spin systems.
Valera, Silvia; Taylor, James E.; Daniels, David S. B.; Dawson, Daniel M.; Athukorala Arachchige, Kasun S.; Ashbrook, Sharon E.; Slawin, Alexandra M. Z.; Bode, Bela E.; The Journal of organic chemistry 79 (2014) 8313–8323; doi:10.1021/jo5015678

data_4029884
_publ_section_title
;
 A modular approach for the synthesis of nanometer-sized polynitroxide
 multi-spin systems.
;
_journal_issue                   17
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              8313
_journal_page_last               8323
_journal_paper_doi               10.1021/jo5015678
_journal_volume                  79
_journal_year                    2014
_chemical_formula_moiety         'C33 H42 N3 O9'
_chemical_formula_sum            'C33 H42 N3 O9'
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_symmetry_cell_setting           triclinic
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_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
_cell_angle_alpha                78.32(3)
_cell_angle_beta                 76.694(19)
_cell_angle_gamma                73.73(3)
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_cell_length_a                   12.594(3)
_cell_length_b                   15.145(2)
_cell_length_c                   19.256(5)
_cell_measurement_reflns_used    7149
_cell_measurement_temperature    93
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      1.66
_cell_volume                     3393.5(14)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 rc13'
_computing_data_collection
'CrystalClear-SM Expert 2.0 rc13 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 rc13'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'Superflip (Palatinus, et al., 2007)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 14.629
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0979
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
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_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22033
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.961
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_diffrn_reflns_theta_max         25.311
_diffrn_reflns_theta_min         1.099
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.242
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
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_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.150
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_refine_ls_extinction_method     none
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_refine_ls_number_parameters     838
_refine_ls_number_reflns         11894
_refine_ls_number_restraints     14
_refine_ls_R_factor_gt           0.1029
_refine_ls_shift/su_max          0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1589P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.3423
_reflns_number_gt                5317
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_cod_data_source_file            jo5015678_si_003.cif
_cod_data_source_block           9
_cod_depositor_comments
'Adding full bibliography for 4029884--4029885.cif.'
_cod_original_cell_volume        3393.3(12)
_cod_database_code               4029884