Conformational and spectroscopic properties of p-extended, bipyrrole-fused rubyrin and sapphyrin derivatives
Se-Young Kee; Jong Min Lim; Soo-Jin Kim; Jaeduk Yoo; Jung-Su Park; Tridib Sarma; Vincent M. Lynch; Pradeepta K. Panda; Jonathan L. Sessler; Dongho Kim; Chang-Hee Lee; Chem.Commun. 47 (2011) 6813–; doi:10.1039/c1cc11733e

data_7106531
_publ_section_title
;
 Conformational and spectroscopic properties of p-extended,
 bipyrrole-fused rubyrin and sapphyrin derivatives
;
_journal_name_full               Chem.Commun.
_journal_page_first              6813
_journal_paper_doi               10.1039/c1cc11733e
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety
'C64 H20 N6 F20 1+, Cl 1-, 2 C5 H12, 2 C H2 Cl2'
_chemical_formula_sum            'C76 H48 Cl5 F20 N6'
_chemical_formula_weight         1602.45
_chemical_name_systematic
;
?
;
_space_group_IT_number           113
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2ab'
_symmetry_space_group_name_H-M   'P -4 21 m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   21.411(2)
_cell_length_b                   21.411(2)
_cell_length_c                   7.5217(8)
_cell_measurement_reflns_used    3369
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.0
_cell_volume                     3448.2(6)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_structure_refinement  'XL SHELXTL/PC, Siemens Analytical'
_computing_structure_solution
;

SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C.,
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
;
_diffrn_ambient_temperature      233(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Rigaku SCX-Mini with Mercury CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0938
_diffrn_reflns_av_sigmaI/netI    0.0469
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            19139
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    0.316
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Abscor. T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            'light brown'
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1622
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.225
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.182
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         1742
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.184
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0636P)^2^+0.6758P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1248
_refine_ls_wR_factor_ref         0.1409
_reflns_number_gt                1195
_reflns_number_total             1742
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc11733e.txt
_cod_data_source_block           Naphtharubyrin
_cod_original_cell_volume        3448.2(7)
_cod_database_code               7106531