Direct observation of deuterium migration in crystalline-state reaction by single-crystal neutron diffraction. III. Photoracemization of 1-cyanoethyl cobaloxime complexes
Ohhara, Takashi; Uekusa, Hidehiro; Ohashi, Yuji; Tanaka, Ichiro; Kumazawa, Shintaro; Niimura, Nobuo; Acta Crystallographica Section B 57 (2001) 551–559; doi:10.1107/S0108768101006838

data_2103706
_publ_section_title
;
 Direct observation of deuterium migration in crystalline-state
 reaction by single-crystal neutron diffraction. III. Photoracemization
 of 1-cyanoethyl cobaloxime complexes
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              551
_journal_page_last               559
_journal_paper_doi               10.1107/S0108768101006838
_journal_volume                  57
_journal_year                    2001
_chemical_formula_sum            'C16 H28 Co D N6 O4'
_chemical_formula_weight         429.38
_chemical_name_systematic
;
[(R,S)-1-cyanoethyl](piperidine)bis(dimethylglyoximato)cobalt(III)
 irradiated
;
_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'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.4039(2)
_cell_length_b                   11.73540(10)
_cell_length_c                   30.7446(2)
_cell_measurement_reflns_used    '512 (determined by X-ray)'
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      '35.00 (X-ray, MoK\a)'
_cell_measurement_theta_min      '1.86 (X-ray, MoK\a)'
_cell_volume                     4114.53(8)
_computing_cell_refinement       'local program'
_computing_data_collection       'local program'
_computing_data_reduction        'local program'
_computing_molecular_graphics    ORTEPIII
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'initial structure was determined by X-ray'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full .291
_diffrn_measured_fraction_theta_max .291
_diffrn_measurement_device_type  BIX-I
_diffrn_measurement_method       '0.2deg \w step scan'
_diffrn_radiation_monochromator  'bent Si crystal'
_diffrn_radiation_probe          neutron
_diffrn_radiation_source         'JRR-3M atomic reactor'
_diffrn_radiation_type           Neutron
_diffrn_radiation_wavelength     1.06000
_diffrn_reflns_av_R_equivalents  .0631
_diffrn_reflns_av_sigmaI/netI    .0522
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            2928
_diffrn_reflns_theta_full        43.58
_diffrn_reflns_theta_max         43.58
_diffrn_reflns_theta_min         1.98
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    .244
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    .730
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             72
_exptl_crystal_size_max          3.0
_exptl_crystal_size_mid          3.0
_exptl_crystal_size_min          1.0
_refine_diff_density_max         .106
_refine_diff_density_min         -.084
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     805
_refine_ls_number_reflns         2137
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          .1043
_refine_ls_R_factor_gt           .1036
_refine_ls_shift/su_max          .056
_refine_ls_shift/su_mean         .009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2309P)^2^+0.6072P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .2680
_reflns_number_gt                2124
_reflns_number_total             2137
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            bs0016.cif
_cod_data_source_block           3-neutron
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P21 21 21'
_cod_database_code               2103706
_cod_database_fobs_code          2103706