Synthesis and Structural Characterization of Porphyrinic Enediynes: Geometric and Electronic Effects on Thermal and Photochemical Reactivity
Tilak Chandra; Brian J. Kraft; John C. Huffman; Jeffrey M. Zaleski; Inorganic Chemistry 42 (2003) 5158–5172; doi:10.1021/ic030035a

data_4314005
_publ_section_title
;
 Synthesis and Structural Characterization of Porphyrinic Enediynes:
 Geometric and Electronic Effects on Thermal and Photochemical Reactivity
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5158
_journal_page_last               5172
_journal_paper_doi               10.1021/ic030035a
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C80 H64 Cl3 N5.33'
_chemical_formula_weight         1206.38
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           4
_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                 95.289(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            3
_cell_length_a                   14.962(3)
_cell_length_b                   16.981(3)
_cell_length_c                   15.520(3)
_cell_measurement_reflns_used    7096
_cell_measurement_temperature    82(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.17
_cell_volume                     3926.4(13)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999), XTEL (local package)'
_computing_molecular_graphics    'Local programs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      82(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
'   0.30 degree frames measured for  64.59 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       '\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  0.0976
_diffrn_reflns_av_sigmaI/netI    0.1303
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20691
_diffrn_reflns_theta_full        27.73
_diffrn_reflns_theta_max         27.73
_diffrn_reflns_theta_min         2.17
_diffrn_standards_interval_time  656
_exptl_absorpt_coefficient_mu    0.237
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelop
_exptl_crystal_F_000             1897
_exptl_crystal_size_max          .11
_exptl_crystal_size_mid          .18
_exptl_crystal_size_min          .26
_refine_diff_density_max         0.973
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.129
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.25(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1063
_refine_ls_number_reflns         13421
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1661
_refine_ls_R_factor_gt           0.1152
_refine_ls_shift/su_max          0.084
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2942
_refine_ls_wR_factor_ref         0.3256
_reflns_number_gt                7963
_reflns_number_total             13421
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic030035a_5.cif
_cod_data_source_block           c:\2002data\02012lb\final
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4314005