Electron acceptors of the fluorene series. Part 13. 9-(5-Nitrofuran-2-ylidene)- and 9-(5-nitro-2-thienylidene)-2,4,5,7-tetranitrofluorenes: novel π-extended electron acceptors. Synthesis, cyclic voltammetry and X-ray crystal structures for the acceptor and its 4,5-dimethyltetrathiafulvalene complex, and a theoretical study†
Perepichka, Igor F.; Perepichka, Dmitrii F.; Lyubchik, Svetlana B.; Bryce, Martin R.; Batsanov, Andrei S.; Howard, Judith A. K.; Journal of the Chemical Society, Perkin Transactions 2  (2001) 1546–; doi:10.1039/b103392c

data_7216984
_publ_section_title
;
 Electron acceptors of the fluorene series. Part 13.
 9-(5-Nitrofuran-2-ylidene)- and
 9-(5-nitro-2-thienylidene)-2,4,5,7-tetranitrofluorenes: novel \p-extended
 electron acceptors. Synthesis, cyclic voltammetry and X-ray crystal
 structures for the acceptor and its 4,5-dimethyltetrathiafulvalene
 complex, and a theoretical study&#x2020;
;
_journal_issue                   9
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 2'
_journal_page_first              1546
_journal_paper_doi               10.1039/b103392c
_journal_year                    2001
_chemical_formula_moiety         'C18 H7 N5 O11,(C4 H8 O2)2'
_chemical_formula_sum            'C26 H23 N5 O15'
_chemical_formula_weight         645.49
_chemical_name_systematic
; 
9-(5-nitrofuran-2-ylidene)-2,4,5,7-tetranitrofluorene: dioxane (1:2) 
;
_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                 109.43(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.588(5)
_cell_length_b                   8.667(3)
_cell_length_c                   21.798(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.3
_cell_measurement_theta_min      15.6
_cell_volume                     2777.2(14)
_computing_cell_refinement       AFC/MSC
_computing_data_collection       AFC/MSC
_computing_data_reduction        TEXSAN
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Rigaku AFC6S 4-circle diffractometer'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            3426
_diffrn_reflns_theta_full        49.99
_diffrn_reflns_theta_max         49.99
_diffrn_reflns_theta_min         3.06
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.120
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8493
_exptl_absorpt_process_details   'T_max,min from psi-scans'
_exptl_crystal_colour            amber
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.216
_refine_diff_density_min         -0.180
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       0.00099(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         2770
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+1.2514P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.0968
_reflns_number_gt                2236
_reflns_number_total             2770
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b103392c.txt
_cod_data_source_block           2a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7216984