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_4114161
_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            'C48 H24 Br2 N4 Ni'
_chemical_formula_weight         875.24
_chemical_name_systematic
; 
  ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             08/15/2002
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   26.8378(15)
_cell_length_b                   7.2109(4)
_cell_length_c                   34.9225(18)
_cell_measurement_reflns_used    6479
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.83
_cell_measurement_theta_min      2.54
_cell_volume                     6758.4(6)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
'   0.30 degree frames measured for  64.63 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  0.1905
_diffrn_reflns_av_sigmaI/netI    0.2016
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            52199
_diffrn_reflns_theta_full        30.06
_diffrn_reflns_theta_max         30.06
_diffrn_reflns_theta_min         2.56
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    2.985
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.720
_exptl_crystal_description       needle
_exptl_crystal_F_000             3504
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.896
_refine_diff_density_min         -0.776
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.792
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         9859
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.792
_refine_ls_R_factor_all          0.1584
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0953
_reflns_number_gt                4224
_reflns_number_total             9859
_reflns_threshold_expression     2sigma(I)
_cod_data_source_file            ja0302782_1.cif
_cod_data_source_block           MSC02073
_cod_database_code               4114161