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_4314002
_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            'C96 H60 Cl8 N4 Ni'
_chemical_formula_weight         1611.87
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method
'minor manual editing of SDT2CIF v. 1.2 BETA  output'
_cell_angle_alpha                102.745(4)
_cell_angle_beta                 96.614(4)
_cell_angle_gamma                104.401(3)
_cell_formula_units_Z            2
_cell_length_a                   13.8989(17)
_cell_length_b                   15.519(2)
_cell_length_c                   19.022(2)
_cell_measurement_reflns_used    7425
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.36
_cell_volume                     3812.8(8)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999), XTEL (local package)'
_computing_molecular_graphics    'XTEL, local package'
_computing_publication_material  'XTEL, local package'
_computing_structure_refinement  'XTEL, local package'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measurement_details
'   0.30 degree frames measured for  30.16 seconds each'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.055
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            65161
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         2.67
_diffrn_standards_decay_%        0.
_diffrn_standards_interval_time  1220
_diffrn_standards_number         7426
_exptl_absorpt_coefficient_mu    0.5878
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular plate'
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          .35
_exptl_crystal_size_mid          .20
_exptl_crystal_size_min          .08
_refine_diff_density_max         0.99
_refine_diff_density_min         -0.82
_refine_ls_abs_structure_details none
_refine_ls_extinction_coef       -0.00000018(3)
_refine_ls_extinction_expression
;
Larson, A. C. (1967).  Acta Cryst. 23, p. 664.  Eq. (3)
;
_refine_ls_extinction_method     Zachariasen
_refine_ls_goodness_of_fit_ref   1.864
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     988
_refine_ls_number_reflns         8716
_refine_ls_R_factor_gt           0.0653
_refine_ls_shift/su_max          0.02
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w^-1^=\s^2^(F)+(.07F)^2^
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0569
_reflns_number_gt                8716
_reflns_number_total             17469
_reflns_threshold_expression     'gt. 2.33*sigma'
_cod_data_source_file            ic030035a_2.cif
_cod_data_source_block           MSC01138
_cod_original_cell_volume        3812.9(9)
_cod_original_formula_sum        'C96 H60 Cl8 N4 Ni1'
_cod_database_code               4314002