Side Chain Entropy and the Activation of Organocobalamins for Carbon-Cobalt Bond Homolysis: Synthesis, Characterization, and Thermolysis of the Neopentyl Derivative of a Unique Cobalamin Analog Lacking a c Side Chain
Kenneth L. Brown; Shifa Cheng; Jeffrey D. Zubkowski; Edward J. Valente; Inorganic Chemistry 36 (1997) 1772–1781; doi:10.1021/ic961378u

data_4323394
_publ_section_title
;
 Side Chain Entropy and the Activation of Organocobalamins for
 Carbon-Cobalt Bond Homolysis: Synthesis, Characterization, and
 Thermolysis of the Neopentyl Derivative of a Unique Cobalamin Analog
 Lacking a c Side Chain
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1772
_journal_page_last               1781
_journal_paper_doi               10.1021/ic961378u
_journal_volume                  36
_journal_year                    1997
_chemical_compound_source        'Brown (Ohio University)'
_chemical_formula_sum            'C64 H127 Co N12 O31 P'
_chemical_formula_weight         1650.68
_chemical_name_common            'Cyanocobalamin 8-butanamide'
_chemical_name_systematic
; 
Cyanocobalamin 8-butanamide hydrate
;
_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'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.041(11)
_cell_length_b                   21.936(15)
_cell_length_c                   25.430(16)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      12
_cell_volume                     8948(10)
_computing_cell_refinement       'P3(Siemens Analytical X-ray Inc.)'
_computing_data_collection       'P3(Siemens Analytical X-ray Inc.)'
_computing_data_reduction        'XDISK (Siemens Anaytical X-ray Inc.)'
_computing_molecular_graphics    'XP (Siemens Analytical X-ray Inc.)'
_computing_publication_material  'SHELXL (Sheldrick, George)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'scintillation counter (PHA)'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_sigmaI/netI    0.2130
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7310
_diffrn_reflns_theta_max         22.48
_diffrn_reflns_theta_min         1.76
_diffrn_standards_decay_%        7.2
_diffrn_standards_interval_count 97
_diffrn_standards_interval_time  1.0h
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.290
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    NA
_exptl_crystal_description       Prisms
_exptl_crystal_F_000             3540
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(4)
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.713
_refine_ls_goodness_of_fit_obs   1.137
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     996
_refine_ls_number_reflns         6401
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      0.737
_refine_ls_restrained_S_obs      1.165
_refine_ls_R_factor_all          0.1147
_refine_ls_R_factor_obs          0.0554
_refine_ls_shift/esd_max         -0.006
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0383P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1207
_refine_ls_wR_factor_obs         0.1083
_reflns_number_observed          2682
_reflns_number_total             6401
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961378u.cif
_cod_data_source_block           C64H127CoN12O31P
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'NA' 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^)+(0.0383P)^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^)+(0.0383P)^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        8948.2(103)
_cod_database_code               4323394