Octaalkyl tetracene-1,2,3,4,7,8,9,10-octacarboxylates: synthesis by twofold [2+2+2] cocyclization and crystallochromy
Chitoshi Kitamura; Akira Takenaka; Takeshi Kawase; Takashi Kobayashi; Hiroyoshi Naito;; Chem.Commun.  (2011) 6653–; doi:10.1039/c1cc11655j

data_7106507
_publ_section_title
;
 Octaalkyl tetracene-1,2,3,4,7,8,9,10-octacarboxylates: synthesis by
 twofold [2+2+2] cocyclization and crystallochromy
;
_journal_name_full               Chem.Commun.
_journal_page_first              6653
_journal_paper_doi               10.1039/c1cc11655j
_journal_year                    2011
_chemical_formula_moiety         'C50 H60 O16'
_chemical_formula_sum            'C50 H60 O16'
_chemical_formula_weight         916.98
_chemical_melting_point          428
_chemical_name_common
'Octapropyl tetracene-1,2,3,4,7,8,9,10-octacarboxylate'
_chemical_name_systematic
;
Octapropyl tetracene-1,2,3,4,7,8,9,10-octacarboxylate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2010-08-05
_audit_creation_method           WinGX
_cell_angle_alpha                72.313(4)
_cell_angle_beta                 73.227(4)
_cell_angle_gamma                73.558(4)
_cell_formula_units_Z            1
_cell_length_a                   9.570(2)
_cell_length_b                   10.081(2)
_cell_length_c                   13.754(2)
_cell_measurement_reflns_used    5718
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.415
_cell_measurement_theta_min      2.99
_cell_measurement_wavelength     0.71073
_cell_volume                     1182.3(4)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 2006)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 2006)'
_computing_data_reduction        'RAPID-AUTO (Rigaku, 2006)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Giacovazzo et al, 2005)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku R-Axis Rapid'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0823
_diffrn_reflns_av_unetI/netI     0.0824
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19549
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.99
_diffrn_source                   'fine-focus sealed x-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         5390
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.1546
_refine_ls_R_factor_gt           0.0805
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1284P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2098
_refine_ls_wR_factor_ref         0.2587
_reflns_number_gt                2397
_reflns_number_total             5390
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c1cc11655j.txt
_cod_data_source_block           pret
_cod_database_code               7106507