Direct Observation of Deuterium Migration in Crystalline-State Reaction by Single Crystal Neutron Diffraction II. 3-1 Photoisomerization of a Cobaloxime Complex
Ohhara, Takashi; Harada, Jun; Ohashi, Yuji; Tanaka, Ichiro; Kumazawa, Shintaro; Niimura, Nobuo; Acta Crystallographica, Section B 56 (2000) 245–253; doi:10.1107/S0108768199012008

data_2102054
_publ_section_title
;
Direct Observation of Deuterium Migration in Crystalline-State
Reaction by Single Crystal Neutron Diffraction II.
3-1 Photoisomerization of a Cobaloxime Complex
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica, Section B'
_journal_page_first              245
_journal_page_last               253
_journal_paper_doi               10.1107/S0108768199012008
_journal_volume                  56
_journal_year                    2000
_chemical_formula_iupac
'[Co (C4 D7 N2 O2)2 (C4 H4 D2 N) (C8 D11 N1)]'
_chemical_formula_sum            'C20 H4 Co D27 N6 O4'
_chemical_formula_weight         504.00
_chemical_name_systematic
;
(3-cyanopropyl)[(R)-1-phenylethylamine]cobaloxime
;
_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                90.000(5)
_cell_angle_beta                 99.9540(10)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            2
_cell_length_a                   9.15790(10)
_cell_length_b                   13.9694(2)
_cell_length_c                   9.27570(10)
_cell_measurement_reflns_used    'not refined'
_cell_measurement_temperature    293(2)
_cell_volume                     1168.78(2)
_computing_cell_refinement       'local program'
_computing_data_collection       'local program'
_computing_data_reduction        'local program'
_computing_molecular_graphics    'ORTEP-III (Burnet & Johnson, 1996)'
_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     1.060
_diffrn_reflns_av_R_equivalents  .0676
_diffrn_reflns_av_sigmaI/netI    .0438
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2540
_diffrn_reflns_theta_max         43.37
_diffrn_reflns_theta_min         3.33
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    .000
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             504
_exptl_crystal_size_max          3.5
_exptl_crystal_size_mid          3.5
_exptl_crystal_size_min          .7
_refine_diff_density_max         .146
_refine_diff_density_min         -.109
_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   1.108
_refine_ls_goodness_of_fit_obs   1.107
_refine_ls_hydrogen_treatment    D-fourier
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         1509
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.106
_refine_ls_restrained_S_obs      1.106
_refine_ls_R_factor_all          .1076
_refine_ls_R_factor_gt           .1065
_refine_ls_shift/esd_max         -.024
_refine_ls_shift/esd_mean        .003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.2366P)^2^+0.1440P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .2853
_reflns_number_observed          1497
_reflns_number_total             1509
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            se0292.cif
_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:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.2366P)^2^+0.1440P] 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^)+( 0.2366P)^2^+0.1440P] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2102054