Utilizing Redox-Mediated Bergman Cyclization toward the Development of Dual-Action Metalloenediyne Therapeutics
Sarah E. Lindahl; Hyunsoo Park; Maren Pink; Jeffrey M. Zaleski; Journal of the American Chemical Society 135 (2013) 3826–3833; doi:10.1021/ja308190q

data_4119437
_publ_section_title
;
 Utilizing Redox-Mediated Bergman Cyclization toward the Development of
 Dual-Action Metalloenediyne Therapeutics
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3826
_journal_page_last               3833
_journal_paper_doi               10.1021/ja308190q
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C34 H24 I4 P2 Pt, C D2 Cl2'
_chemical_formula_sum            'C35 H24 Cl2 D2 I4 P2 Pt'
_chemical_formula_weight         1282.09
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 97.745(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.8186(15)
_cell_length_b                   17.1433(18)
_cell_length_c                   16.8761(19)
_cell_measurement_reflns_used    9887
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.30
_cell_measurement_theta_min      2.44
_cell_volume                     3674.7(7)
_computing_cell_refinement       'APEX II v2010.11.3 (Bruker, 2010)'
_computing_data_collection       'APEX II v2010.11.3 (Bruker, 2010)'
_computing_data_reduction        'APEX II v2010.11.3 (Bruker, 2010)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2010)'
_computing_publication_material  'SHELXTL (Bruker, 2010)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2010)'
_computing_structure_solution    'SIR-2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 83.33
_diffrn_detector_type            'Bruker APEXII'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
'0.30 degree frames measured for 15 seconds each'
_diffrn_measurement_device       'APEX Kappa Duo'
_diffrn_measurement_device_type  Kappa
_diffrn_measurement_method       'omega and phi 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  0.0571
_diffrn_reflns_av_sigmaI/netI    0.0370
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            55538
_diffrn_reflns_theta_full        26.55
_diffrn_reflns_theta_max         26.55
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    7.436
_exptl_absorpt_correction_T_max  0.7075
_exptl_absorpt_correction_T_min  0.2915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing; 1995'
_exptl_crystal_colour            beige
_exptl_crystal_density_diffrn    2.317
_exptl_crystal_description       plate
_exptl_crystal_F_000             2360
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.566
_refine_diff_density_min         -1.627
_refine_diff_density_rms         0.208
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         7591
_refine_ls_number_restraints     119
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0369P)^2^+12.6475P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0863
_reflns_number_gt                6288
_reflns_number_total             7591
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja308190q_si_002.cif
_cod_data_source_block           11039
_cod_database_code               4119437