Serendipitous synthetic entrée to tetradehydro analogues of cobalamins
Deans, Richard M.; Mass, Olga; Diers, James R.; Bocian, David F.; Lindsey, Jonathan S.; New Journal of Chemistry 37 (2013) 3964–; doi:10.1039/c3nj00574g

data_7053239
_publ_section_title
;
 Serendipitous synthetic entr\'ee to tetradehydro analogues of cobalamins
;
_journal_issue                   12
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3964
_journal_paper_doi               10.1039/c3nj00574g
_journal_volume                  37
_journal_year                    2013
_chemical_formula_sum            'C39.07 H42.07 Cl0.22 N4'
_chemical_formula_weight         575.59
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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            16
_cell_length_a                   30.805(7)
_cell_length_b                   30.805(7)
_cell_length_c                   14.937(3)
_cell_measurement_reflns_used    9730
_cell_measurement_temperature    110
_cell_measurement_theta_max      30.54
_cell_measurement_theta_min      2.41
_cell_volume                     14174(5)
_computing_cell_refinement       SAINT
_computing_data_collection       Apex2
_computing_data_reduction        SAINT
_computing_molecular_graphics    NRCVAX
_computing_publication_material  cif2tables.py
_computing_structure_refinement  XL
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker-Nonius Kappa Axis X8 Apex2'
_diffrn_measurement_method       'omega and phi scans'
_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  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0389
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            157107
_diffrn_reflns_theta_full        32.52
_diffrn_reflns_theta_max         33.79
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_T_max  0.9711
_exptl_absorpt_correction_T_min  0.9613
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.079
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4933
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.37
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.232
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         13754
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0963
_refine_ls_R_factor_gt           0.0530
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0772P)^2^+3.7230P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1321
_refine_ls_wR_factor_ref         0.1543
_reflns_number_gt                8823
_reflns_number_total             13754
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3nj00574g.txt
_cod_data_source_block           x12117
_cod_original_cell_volume        14174(4)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7053239