Direct Observation of Deuterium Migration in Crystalline-State Reaction by Single Crystal Neutron Diffraction IV. "Hula-Twist" Rotation of a Long Alkyl Radical Produced by Photoirradiation
Takashi Ohhara; Susumu Ikeda; Hiroyuki Imura; Hidehiro Uekusa; Yuji Ohashi; Ichiro Tanaka; Nobuo Niimura; Journal of the American Chemical Society 124 (2002) 14736–14740; doi:10.1021/ja027872g

data_4115367
_publ_section_title
;
 Direct Observation of Deuterium Migration in Crystalline-State Reaction
 by Single Crystal Neutron Diffraction IV. "Hula-Twist" Rotation of a Long
 Alkyl Radical Produced by Photoirradiation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14736
_journal_page_last               14740
_journal_paper_doi               10.1021/ja027872g
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C21 H14 Co D18 N5 O8'
_chemical_formula_weight         559.6
_chemical_name_systematic
; 
[(R)-1,2-bis(ethoxycarbonyl)ethyl-d1a](pyridine-d5)-
bis(dimethylglyoxymato-d6)cobalt(III)
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.121(7)
_cell_length_b                   16.772(10)
_cell_length_c                   16.949(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      14
_cell_volume                     2593(3)
_computing_data_reduction        teXsan
_computing_molecular_graphics    teXsan
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97(Altomare et al., 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       2\q-\w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotate anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0200
_diffrn_reflns_av_sigmaI/netI    0.0168
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5505
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         2.54
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 300
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.714
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_description       plate
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         4289
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0589P)^2^+1.1927P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1065
_refine_ls_wR_factor_ref         0.1133
_reflns_number_gt                3818
_reflns_number_total             4289
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja027872g-2_s1_1.cif
_cod_data_source_block           xray
_cod_original_formula_sum        'C21 H14 Co N5 O8 D18'
_cod_database_code               4115367