Anhydrous TEMPO-H: reactions of a good hydrogen atom donor with low-valent carbon centres.
Giffin, Nick A.; Makramalla, Miller; Hendsbee, Arthur D.; Robertson, Katherine N.; Sherren, Cody; Pye, Cory C.; Masuda, Jason D.; Clyburne, Jason A. C.; Organic & biomolecular chemistry 9 (2011) 3672–3680; doi:10.1039/c0ob00999g

data_7151799
_publ_section_title
;
 Anhydrous TEMPO-H: reactions of a good hydrogen atom donor with
 low-valent carbon centres.
;
_journal_issue                   10
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              3672
_journal_page_last               3680
_journal_paper_doi               10.1039/c0ob00999g
_journal_volume                  9
_journal_year                    2011
_chemical_formula_moiety         'C21 H24 N2, C9 H19 N O'
_chemical_formula_sum            'C30 H43 N3 O'
_chemical_formula_weight         461.67
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 94.250(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.989(2)
_cell_length_b                   15.262(3)
_cell_length_c                   16.648(4)
_cell_measurement_reflns_used    5971
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.29
_cell_volume                     2784.4(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0423
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22240
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.77
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6662
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; BRUKER 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.101
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.232
_exptl_crystal_size_mid          0.189
_exptl_crystal_size_min          0.177
_refine_diff_density_max         0.273
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         6707
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0475
_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^)+(0.0544P)^2^+0.8331P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1140
_refine_ls_wR_factor_ref         0.1271
_reflns_number_gt                4955
_reflns_number_total             6707
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0ob00999g.txt
_cod_data_source_block           unsaturatedIMes-TEMPO-H
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 
;
_cod_original_cell_volume        2784.5(10)
_cod_original_sg_symbol_Hall     '-P 2yn '
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7151799