The highly saddled octaethyltetraphenylporphyrin-[H~4~OETPP] dichloride toluene 1.33-solvate
Hu, Chuanjiang; Noll, Bruce C.; Scheidt, W. Robert.; Acta Crystallographica Section E 63 (2007) o3128–o3128; doi:10.1107/S1600536807027018

data_2214374
_publ_section_title
;
 The highly saddled octaethyltetraphenylporphyrin-[H~4~OETPP]
 dichloride toluene 1.33-solvate
;
_journal_coeditor_code           PK2027
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3128
_journal_page_last               o3128
_journal_paper_doi               10.1107/S1600536807027018
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C60 H64 N4 2+, 2Cl -, 1.33C7 H8'
_chemical_formula_moiety         'C60 H64 N4 2+, 2(Cl -), 1.33(C7 H8)'
_chemical_formula_sum            'C69.33 H74.67 Cl2 N4'
_chemical_formula_weight         1034.90
_chemical_name_common            H~4~OETPP2Cl
_chemical_name_systematic
;
2,3,7,8,12,13,17,18-octaethyl-5,10,15,20-tetraphenylporphyrin dichloride
toluene 1.33-solvate
;
_space_group_IT_number           220
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'I -4bd 2c 3'
_symmetry_space_group_name_H-M   'I -4 3 d'
_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            12
_cell_length_a                   25.8135(2)
_cell_length_b                   25.8135(2)
_cell_length_c                   25.8135(2)
_cell_measurement_reflns_used    9107
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.0
_cell_measurement_theta_min      2.2
_cell_volume                     17200.5(2)
_computing_cell_refinement       'APEX2 and SAINT (Bruker--Nonius, 2004)'
_computing_data_collection       'APEX2 (Bruker--Nonius, 2004)'
_computing_data_reduction        'SAINT and XPREP (Sheldrick, 2005)'
_computing_molecular_graphics
'XP (Sheldrick, 1998) and PLATON (Spek, 2003)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX II CCD area-detector'
_diffrn_measurement_method       '\f and \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  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0106
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            176336
_diffrn_reflns_theta_full        30.58
_diffrn_reflns_theta_max         30.6
_diffrn_reflns_theta_min         1.9
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.16
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6632
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.29
_refine_diff_density_max         .42
_refine_diff_density_min         -.20
_refine_ls_abs_structure_details 'Flack (1983), 2073 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.07(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.15
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4414
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.14
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0734P)^2^+9.3007P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.119
_refine_ls_wR_factor_ref         0.139
_reflns_number_gt                3859
_reflns_number_total             4414
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            pk2027.cif
_cod_data_source_block           I
_cod_database_code               2214374
_cod_database_fobs_code          2214374