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_2103703
_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 H22 Co D N6 O4'
_chemical_formula_weight         423.33
_chemical_name_systematic
;
 [(R)-1-cyanoethyl](pyridine)bis(dimethylglyoximato)cobalt(III) irradiated
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 94.23(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.023(5)
_cell_length_b                   12.627(2)
_cell_length_c                   9.628(2)
_cell_measurement_reflns_used    '25 (determined by X-rays)'
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      '15 (X-ray, MoK\a)'
_cell_measurement_theta_min      '14 (X-ray, MoK\a)'
_cell_volume                     1942.7(8)
_computing_cell_refinement       'local program'
_computing_data_collection       'local program'
_computing_data_reduction        'local program'
_computing_molecular_graphics    ORTEPIII
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'initial structure was determined by X-ray'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       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  .0763
_diffrn_reflns_av_sigmaI/netI    .0517
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       2
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            1954
_diffrn_reflns_theta_max         41.95
_diffrn_reflns_theta_min         3.07
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    .208
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    .752
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             108
_exptl_crystal_size_max          3.0
_exptl_crystal_size_mid          3.0
_exptl_crystal_size_min          .6
_refine_diff_density_max         .157
_refine_diff_density_min         -.099
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -10(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   3.303
_refine_ls_goodness_of_fit_obs   3.311
_refine_ls_hydrogen_treatment    refine
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         1424
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      3.273
_refine_ls_restrained_S_obs      3.281
_refine_ls_R_factor_all          .1321
_refine_ls_R_factor_obs          .1320
_refine_ls_shift/esd_max         -.136
_refine_ls_shift/esd_mean        .016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .3278
_refine_ls_wR_factor_obs         .3276
_reflns_number_observed          1418
_reflns_number_total             1424
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            bs0016.cif
_cod_data_source_block           2-neutron
_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 1527 2010-12-29 10:47:43Z saulius 

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_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'.
New tag '_refine_ls_weighting_details' was created. The value of the
new tag was set to 'w=1/[s^2^(Fo^2^)+( 0.1000P)^2^+0.0000P] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1942.6(7)
_cod_original_sg_symbol_H-M      P21
_cod_database_code               2103703
_cod_database_fobs_code          2103703