Ambient Temperature Activation of Haloporphyrinic-Enediynes: Electronic Contributions to Bergman Cycloaromatization
Mahendra Nath; John C. Huffman; Jeffrey M. Zaleski; Journal of the American Chemical Society 125 (2003) 11484–11485; doi:10.1021/ja0302782

data_4114164
_publ_contact_author_name        'J. C. Huffman'
_publ_section_title
;
 Ambient Temperature Activation of Haloporphyrinic-Enediynes: Electronic
 Contributions to Bergman Cycloaromatization
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11484
_journal_page_last               11485
_journal_paper_doi               10.1021/ja0302782
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C105 H59 Cl2 N8 Ni2'
_chemical_formula_weight         1620.92
_chemical_name_systematic
; 
  ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 95.371(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   7.3867(6)
_cell_length_b                   27.458(2)
_cell_length_c                   36.005(3)
_cell_measurement_reflns_used    7017
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.80
_cell_volume                     7270.6(10)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999), XTEL (local package)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
'   0.30 degree frames measured for  10.14 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  0.0962
_diffrn_reflns_av_sigmaI/netI    0.0660
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            108318
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.26
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.655
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_description       'cleaved needle'
_exptl_crystal_F_000             3340
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.154
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1259
_refine_ls_number_reflns         16715
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1022
_refine_ls_R_factor_gt           0.0656
_refine_ls_shift/su_max          0.069
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1232P)^2^+0.1561P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1910
_refine_ls_wR_factor_ref         0.2123
_reflns_number_gt                10867
_reflns_number_total             16715
_reflns_threshold_expression     2sigma(I)
_cod_data_source_file            ja0302782_4.cif
_cod_data_source_block           03010
_cod_original_cell_volume        7270.7(10)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4114164