Strong Trans Influence Methoxymethyl Ligand in B12 Cobaloxime and Imine/Oxime Model Complexes: Structural, Spectroscopic, and Molecular Mechanics Investigations
Renzo Cini; Scott J. Moore; Luigi G. Marzilli; Inorganic Chemistry 37 (1998) 6890–6897; doi:10.1021/ic980666i

data_4323252
_publ_section_title
;
 Strong Trans Influence Methoxymethyl Ligand in B12 Cobaloxime and
 Imine/Oxime Model Complexes: Structural, Spectroscopic, and Molecular
 Mechanics Investigations
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6890
_journal_page_last               6897
_journal_paper_doi               10.1021/ic980666i
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C20.6 H33.4 Co N6 O5.6'
_chemical_formula_weight         513.66
_chemical_name_common
1,5,6-trimethylbenzimidazole-methoxymethylcobaloxime
_chemical_name_systematic
; 

trans-bis(Dimethylglyoximato)-methoxymethyl-(1,5,6-trimethylbenzimidazole)-c
obalt(iii)
;
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 94.240(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.1150(10)
_cell_length_b                   15.8670(10)
_cell_length_c                   19.266(2)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      10
_cell_volume                     2473.9(4)
_computing_cell_refinement       XSCAN
_computing_data_collection       XSCAN
_computing_data_reduction        XSCAN
_computing_molecular_graphics    'ZORTEP, (SZOLNAY, Heidelberg, 1995) '
_computing_publication_material  'SHELX-93 CIFTAB '
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       SIEMENS-P4
_diffrn_measurement_method       omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_sigmaI/netI    0.0146
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            4657
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        0.02
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.738
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_density_meas      ?
_exptl_crystal_description       y
_exptl_crystal_F_000             1083
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.663
_refine_diff_density_min         -0.232
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       n
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.105
_refine_ls_goodness_of_fit_obs   1.143
_refine_ls_hydrogen_treatment    y
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         4316
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.136
_refine_ls_restrained_S_obs      1.143
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_obs          0.0393
_refine_ls_shift/esd_max         0.857
_refine_ls_shift/esd_mean        0.175
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0696P)^2^+1.7590P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1311
_refine_ls_wR_factor_obs         0.1215
_reflns_number_observed          3698
_reflns_number_total             4333
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980666i_1.cif
_cod_data_source_block           Me3BzmCo(DH)2CH2OCH3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0696P)^2^+1.7590P] 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^)+(0.0696P)^2^+1.7590P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C20.60 H33.40 Co N6 O5.60'
_cod_database_code               4323252