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_2103704
_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 H29 Co N6 O4'
_chemical_formula_weight         428.38
_chemical_name_systematic
;
 [(R,S)-1-cyanoethyl](piperidine)bis(dimethylglyoximato)cobalt(III) initial
;
_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                   11.4309(12)
_cell_length_b                   11.6591(6)
_cell_length_c                   30.701(3)
_cell_measurement_reflns_used    512
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      1.33
_cell_volume                     4091.6(6)
_computing_cell_refinement       'SAINT (Siemens, 1994)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1994)'
_computing_molecular_graphics    ORTEPIII
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Cascarano et al., 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full .892
_diffrn_measured_fraction_theta_max .892
_diffrn_measurement_device_type  'Bluker SMART CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotate anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .1135
_diffrn_reflns_av_sigmaI/netI    .0699
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            15591
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         1.33
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    .872
_exptl_absorpt_correction_T_max  .781
_exptl_absorpt_correction_T_min  .632
_exptl_absorpt_correction_type   'empirical (SADABS: Sheldrick, 1996)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          .3
_exptl_crystal_size_mid          .3
_exptl_crystal_size_min          .1
_refine_diff_density_max         .797
_refine_diff_density_min         -1.338
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   .10(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.766
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         8265
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.766
_refine_ls_R_factor_all          .0893
_refine_ls_R_factor_gt           .0837
_refine_ls_shift/su_max          .002
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc 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_ref         .2523
_reflns_number_gt                7379
_reflns_number_total             8265
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            bs0016.cif
_cod_data_source_block           3-initial
_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               2103704
_cod_database_fobs_code          2103704