Synthetic Approaches to Amino Analogues of N-Acetylcolchinol
Virginie Colombel; Olivier Baudoin; Journal of Organic Chemistry 74 (2009) 4329–4335; doi:10.1021/jo900632a

data_4024572
_publ_section_title
;
Synthetic Approaches to Amino Analogues of N-Acetylcolchinol
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              4329
_journal_page_last               4335
_journal_paper_doi               10.1021/jo900632a
_journal_volume                  74
_journal_year                    2009
_chemical_formula_moiety         'C31 H36 N2 O11'
_chemical_formula_sum            'C31 H36 N2 O11'
_chemical_formula_weight         612.63
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             09-03-09
_audit_creation_method           CRYSTALS_ver_12.86
_cell_angle_alpha                91.168(9)
_cell_angle_beta                 105.274(9)
_cell_angle_gamma                90.545(9)
_cell_formula_units_Z            2
_cell_length_a                   9.8130(11)
_cell_length_b                   12.0815(13)
_cell_length_c                   13.4125(14)
_cell_measurement_reflns_used    4279
_cell_measurement_temperature    293
_cell_measurement_theta_max      62.3729
_cell_measurement_theta_min      3.4129
_cell_volume                     1533.4(3)
_computing_cell_refinement       'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean 10.4685
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type
;
Goniometer Xcalibur, detector: Atlas (Gemini ultra Cu)
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.068
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7342
_diffrn_reflns_theta_full        35.660
_diffrn_reflns_theta_max         62.561
_diffrn_reflns_theta_min         3.417
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.848
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.51
_refine_diff_density_min         -0.51
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8889
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         3397
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1022
_refine_ls_R_factor_gt           0.0862
_refine_ls_shift/su_max          0.000216
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 21.9 -7.15 16.6 -1.32 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0950
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0850
_reflns_limit_h_max              10
_reflns_limit_h_min              -11
_reflns_limit_k_max              13
_reflns_limit_k_min              -13
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                3397
_reflns_number_total             4571
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0862
_oxford_refine_ls_scale          5.212(17)
_oxford_reflns_number_all        4547
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_oxford_structure_analysis_title 'vcl531b in P -1'
_cod_data_source_file            jo900632a_si_001.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4024572