Diamidodipyrrins: Versatile Bipyrrolic Ligands with Multiple Metal Binding Modes
Van S. Thoi; Jay R. Stork; Edwards T. Niles; Ezra C. Depperman; David L. Tierney; Seth M. Cohen; Inorganic Chemistry 47 (2008) 10533–10541; doi:10.1021/ic8011876

data_4306337
_publ_contact_author
;      Cohen, Seth M.
       Department of Chemistry and Biochemistry
       University of California, San Diego
       La Jolla
       CA 92093-0358
       USA
;
_publ_contact_author_email       scohen@ucsd.edu
_publ_section_title
;
Diamidodipyrrins: Versatile Bipyrrolic Ligands with Multiple Metal Binding
Modes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10533
_journal_page_last               10541
_journal_paper_doi               10.1021/ic8011876
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety
;
C23 H27 N4 O2, 3(C H Cl3), H2 O, Br
;
_chemical_formula_sum            'C26 H32 Br Cl9 N4 O3'
_chemical_formula_weight         847.52
_chemical_name_common
;
 H~2~DADP^Ph,iPr^Br^.^H~2~O^.^3CHCl~3~ 
;
_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                 94.605(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.987(3)
_cell_length_b                   20.692(5)
_cell_length_c                   25.444(6)
_cell_measurement_reflns_used    9713
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.2
_cell_measurement_theta_min      2.30
_cell_volume                     7340(3)
_computing_cell_refinement       SAINT
_computing_data_collection       'Apex2 v.1.0-2.1 (Bruker, 2006)'
_computing_data_reduction        'SAINT v7.34A (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL 5.1 (Sheldrick, 1994)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker Apex'
_diffrn_measurement_method       \w
_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  0.0545
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            93094
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.27
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.809
_exptl_absorpt_correction_T_max  0.7296
_exptl_absorpt_correction_T_min  0.5235
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.10 (Sheldrick, 2004)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3424
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.264
_refine_diff_density_min         -0.766
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     805
_refine_ls_number_reflns         14795
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0384P)^2^+11.3921P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0898
_refine_ls_wR_factor_ref         0.0987
_reflns_number_gt                11600
_reflns_number_total             14795
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic8011876_si_001_2.cif
_cod_data_source_block           jrs171
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4306337