C-H Bond Activation of Hydrocarbon Segments in Complex Organic Molecules: Total Synthesis of the Antimitotic Rhazinilam
James A. Johnson; Dalibor Sames; Journal of the American Chemical Society 122 (2000) 6321–6322; doi:10.1021/ja0003223

data_4116058
_publ_section_title
;
 C-H Bond Activation of Hydrocarbon Segments in Complex Organic Molecules:
 Total Synthesis of the Antimitotic Rhazinilam
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6321
_journal_page_last               6322
_journal_paper_doi               10.1021/ja0003223
_journal_volume                  122
_journal_year                    2000
_chemical_formula_sum            'C30.5 H32.5 Cl F3 N O5 Pt S'
_chemical_formula_weight         812.68
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 109.7670(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.5434(10)
_cell_length_b                   18.0749(14)
_cell_length_c                   14.1236(11)
_cell_measurement_temperature    233(2)
_cell_volume                     3013.4(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      233(2)
_diffrn_measured_fraction_theta_full 0.911
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0244
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18429
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    4.874
_exptl_absorpt_correction_T_max  0.6414
_exptl_absorpt_correction_T_min  0.1118
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.791
_exptl_crystal_F_000             1602
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.776
_refine_diff_density_min         -3.515
_refine_diff_density_rms         0.153
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.011(8)
_refine_ls_extinction_coef       0.00002(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     775
_refine_ls_number_reflns         8783
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.122
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0726P)^2^+5.5023P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1050
_reflns_number_gt                8309
_reflns_number_total             8783
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0003223.cif
_cod_data_source_block           4
_cod_original_formula_sum        'C30.50 H32.50 Cl F3 N O5 Pt S'
_cod_database_code               4116058