Concise Total Syntheses of (\±)-Strychnine and (\±)-Akuammicine
Gopal Sirasani; Tapas Paul; William Dougherty; Scott Kassel; Rodrigo B. Andrade; Journal of Organic Chemistry 75 (2010) 3529–3532; doi:10.1021/jo100516g

data_4025435
_publ_section_title
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 Concise Total Syntheses of (\+-)-Strychnine and (\+-)-Akuammicine
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              3529
_journal_page_last               3532
_journal_paper_doi               10.1021/jo100516g
_journal_volume                  75
_journal_year                    2010
_chemical_formula_sum            'C21 H25 Cl3 N2 O2'
_chemical_formula_weight         443.78
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.025(4)
_cell_angle_beta                 78.525(4)
_cell_angle_gamma                62.262(3)
_cell_formula_units_Z            2
_cell_length_a                   10.1157(19)
_cell_length_b                   10.700(2)
_cell_length_c                   11.006(2)
_cell_measurement_reflns_used    5803
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.23
_cell_measurement_theta_min      2.68
_cell_volume                     1031.0(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0620
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17124
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         33.36
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.465
_exptl_absorpt_correction_T_max  0.9421
_exptl_absorpt_correction_T_min  0.9294
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.059
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         7832
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1035
_refine_ls_R_factor_gt           0.0625
_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^)+(0.0768P)^2^+0.7847P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1565
_refine_ls_wR_factor_ref         0.1788
_reflns_number_gt                5079
_reflns_number_total             7832
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo100516g_si_002.cif
_cod_data_source_block           andr001
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1030.9(3)
_cod_database_code               4025435