Total synthesis of (+)-kalkitoxin
White, James D.; Lee, Chang-Sun; Xu, Qing; Chemical Communications (Cambridge, United Kingdom)  (2003) 2012–2013; doi:10.1039/b306124h

data_7103851
_publ_section_title
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 Total synthesis of (+)-kalkitoxin
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_journal_coden_ASTM              CHCOFS
_journal_issue                   16
_journal_name_full
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 Chemical Communications (Cambridge, United Kingdom)
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_journal_page_first              2012
_journal_page_last               2013
_journal_paper_doi               10.1039/b306124h
_journal_year                    2003
_chemical_formula_sum            'C26 H33 N O4'
_chemical_formula_weight         423.53
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_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                 102.212(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.048(7)
_cell_length_b                   5.7108(6)
_cell_length_c                   14.709(3)
_cell_measurement_reflns_used    1943
_cell_measurement_theta_max      59.75
_cell_measurement_theta_min      3.09
_cell_volume                     2384.8(8)
_computing_cell_refinement       TwinSolve
_computing_data_collection       CrystalClear
_computing_data_reduction        TwinSolve
_computing_molecular_graphics    'ORTEP-III for windows (Farrugia, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector                 'R-AXIS Rapid IP'
_diffrn_measured_fraction_theta_full 0.888
_diffrn_measured_fraction_theta_max 0.888
_diffrn_measurement_device_type  'R-AXIS-CS3 (RAPID)'
_diffrn_measurement_method       'profile data'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3851
_diffrn_reflns_theta_full        59.51
_diffrn_reflns_theta_max         59.51
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    0.629
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Shape and scale corrections using equivalent reflections.
Shape function based on spherical harmonics.
Highest even and odd order for spherical harmonics:  4  and  1
Laue group:  2/m (b)
Friedel opposites are equivalent.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.249
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.1(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         2613
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0716
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0088P)^2^+14.4336P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1349
_refine_ls_wR_factor_ref         0.1453
_reflns_number_gt                2330
_reflns_number_total             2613
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b306124h.txt
_cod_data_source_block           shelxl
_cod_depositor_comments
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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 
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_cod_original_sg_symbol_H-M      C2
_cod_database_code               7103851