Synthesis and structure of new families of potential antitumor or antiviral agents. I. 4b,6a,10b,10c-Tetrahydrobenzo[3,4]cyclobuta[1,2-<i>a</i>]biphenylene-4b,6a-diyl diacetate
Ianelli, S.; Nardelli, M.; Belletti, D.; Jamart-Grégoire, B.; Mouaddib, A.; Caubère, P.; Acta Crystallographica Section C 49 (1993) 1380–1384; doi:10.1107/S0108270193000265

data_2001547
_publ_section_title
;Synthesis and structure of new families of potential antitumor or antiviral
 agents. I.
 4b,6a,10b,10c-Tetrahydrobenzo[3,4]cyclobuta[1,2-<i>a</i>]biphenylene-4b,6a-diyl
 diacetate
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1380
_journal_page_last               1384
_journal_paper_doi               10.1107/S0108270193000265
_journal_volume                  49
_journal_year                    1993
_chemical_formula_analytical     'C22 H18 O4'
_chemical_formula_sum            'C22 H18 O4'
_chemical_formula_weight         346.38
_chemical_name_systematic
;
4b,6a-bis(acetyloxy)-4b,6a,10b,10c-tetrahydrobenzo[3,4]-cyclo-buta[1,2a]
biphenylene
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 99.100(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9150(10)
_cell_length_b                   19.228(3)
_cell_length_c                   8.0500(10)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      43.4
_cell_measurement_theta_min      25.3
_cell_volume                     1821.1(4)
_computing_cell_refinement       'LQPARM (Nardelli & Mangia, 1984)'
_computing_molecular_graphics    'ORTEP (Johnson, 1965)'
_computing_publication_material  'PARST (Nardelli, 1983)'
_computing_structure_refinement  'SHELX76 (Sheldrick, 1976) and SHELXL92'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens-AED diffractometer'
_diffrn_measurement_method       '\q-2\q scan'
_diffrn_radiation_monochromator  Ni-filter
_diffrn_radiation_source         'standard Cu anode'
_diffrn_radiation_type           'X-ray Cu-K\a mean'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0154
_diffrn_reflns_av_sigmaI/netI    0.0135
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3717
_diffrn_reflns_reduction_process
;
Standard. Lp correction.
;
_diffrn_reflns_theta_max         70.25
_diffrn_reflns_theta_min         3.76
_diffrn_standards_decay_%        'within statistical fluctuation'
_diffrn_standards_interval_count 50
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    .667
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description
;
 tabular prisms
;
_exptl_crystal_F_000             728
_exptl_crystal_size_max          .75
_exptl_crystal_size_mid          .33
_exptl_crystal_size_min          .23
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.197
_refine_ls_extinction_coef       'k = 0.0321(15)'
_refine_ls_extinction_method
;'F~c~^*^ = kF~c~[1+0.001F~c~^2^\l^3^/sin(2\q)]^-1/4^
(SHELXL92; Sheldrick, 1992)
;
_refine_ls_goodness_of_fit_all   1.058
_refine_ls_goodness_of_fit_obs   1.101
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         3456
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.160
_refine_ls_restrained_S_obs      1.101
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_obs          0.0459
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;calc w = 1/[\s^2^(F~o~^2^)+(0.0803P)^2^+0.3073P]
where P = (F~o~^2^+2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1413
_refine_ls_wR_factor_obs         0.1266
_reflns_number_observed          3106
_reflns_number_total             3470
_reflns_observed_criterion       I>2sigma(I)
_cod_data_source_file            ha1033.cif
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2001547