Total synthesis of (±)-rhazinal, an alkaloidal spindle toxin from Kopsia teoi
Banwell, Martin G.; Edwards, Alison J.; Jolliffe, Katrina A.; Smith, Jason A.; Hamel, Ernest; Verdier-Pinard, Pascal; Organic & Biomolecular Chemistry 1 (2003) 296–; doi:10.1039/b209992f

data_7150460
_publ_section_title
;
 Total synthesis of (+-)-rhazinal, an alkaloidal spindle toxin from
 Kopsia teoi
;
_journal_issue                   2
_journal_name_full               'Organic &amp;  Biomolecular Chemistry'
_journal_page_first              296
_journal_paper_doi               10.1039/b209992f
_journal_volume                  1
_journal_year                    2003
_chemical_compound_source        'Local laboratory'
_chemical_formula_moiety         'C20 H22 N2 O2 '
_chemical_formula_sum            'C20 H22 N2 O2'
_chemical_formula_weight         322.408
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   'geom difmap'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             02-09-10
_audit_creation_method           'maXus + CRYSTALS_ver_12-03-99'
_cell_angle_alpha                90.00
_cell_angle_beta                 101.2591(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1081(3)
_cell_length_b                   12.6796(4)
_cell_length_c                   11.6659(4)
_cell_measurement_reflns_used    12226
_cell_measurement_temperature    200
_cell_measurement_theta_max      19.980
_cell_measurement_theta_min      2.910
_cell_volume                     1611.48(9)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001)'
_computing_data_reduction        'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
;
CAMERON (Watkin et al 1996)
;
_computing_publication_material
;
CRYSTALS (Watkin et al 2001) + maXus(Mackay et al., 1999)
;
_computing_structure_refinement
;
CRYSTALS (Watkin et al 2001)
;
_computing_structure_solution
;
SIR97 (Altomare et al, 1999)
;
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.08976
_diffrn_orient_matrix_UB_12      0.01575
_diffrn_orient_matrix_UB_13      0.02211
_diffrn_orient_matrix_UB_21      -0.00899
_diffrn_orient_matrix_UB_22      0.01335
_diffrn_orient_matrix_UB_23      0.08239
_diffrn_orient_matrix_UB_31      0.01699
_diffrn_orient_matrix_UB_32      -0.07612
_diffrn_orient_matrix_UB_33      0.01902
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           ' MoK\a'
_diffrn_radiation_wavelength_id  all
_diffrn_reflns_av_R_equivalents  0.077
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            18571
_diffrn_reflns_theta_max         19.98
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.989
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.59
_refine_diff_density_min         -0.65
_refine_diff_density_rms         0.28
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8346
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     117
_refine_ls_number_reflns         902
_refine_ls_R_factor_gt           0.0973
_refine_ls_shift/su_max          0.000056
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 
1.20    0.175E-010.530    
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0854
_reflns_d_resolution_high        0.72
_reflns_d_resolution_low         1.78
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              11
_reflns_limit_l_min              0
_reflns_number_gt                902
_reflns_number_total             1493
_reflns_threshold_expression     >3.00\s(I)
_cod_data_source_file            b209992f.txt
_cod_data_source_block
;
;
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 21/n'
_cod_original_formula_sum        'C20 H22 N2 O2 '
_cod_database_code               7150460