Reduction-free synthesis of stable acetylide cobalamins
Mikolaj Chrominski; Agnieszka Lewalska; Dorota Gryko; Chem.Commun. 49 (2013) 11406–; doi:10.1039/c3cc47210h

data_7110086
_publ_section_title
;
 Reduction-free synthesis of stable acetylide cobalamins
;
_journal_name_full               Chem.Commun.
_journal_page_first              11406
_journal_paper_doi               10.1039/c3cc47210h
_journal_volume                  49
_journal_year                    2013
_chemical_formula_sum            'C77 H103 Co N13 O25 P'
_chemical_formula_weight         1700.62
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.8339(4)
_cell_length_b                   21.8117(6)
_cell_length_c                   25.9778(7)
_cell_measurement_temperature    173(2)
_cell_volume                     8971.8(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0572
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            44222
_diffrn_reflns_theta_full        67.54
_diffrn_reflns_theta_max         67.54
_diffrn_reflns_theta_min         3.27
_exptl_absorpt_coefficient_mu    2.324
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3592
_refine_diff_density_max         0.986
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.004(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1049
_refine_ls_number_reflns         14407
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0583
_refine_ls_shift/su_max          4.331
_refine_ls_shift/su_mean         0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1293P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1670
_refine_ls_wR_factor_ref         0.1704
_reflns_number_gt                12835
_reflns_number_total             14407
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc47210h.txt
_cod_data_source_block           c:\users\admin\desktop\mik557\nowyfo~1\mik557_0
_cod_database_code               7110086