#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:02:01 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180056 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/02/7050252.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7050252
loop_
_publ_author_name
'Tanaka, Koichi'
'Iwamoto, Toshimasa'
'Caira, Mino R.'
_publ_section_title
;
 Conglomerate and racemate formation of
 2,3-bisfluoren-9-ylidenesuccinic acid by inclusion complexation with
 achiral guest molecules
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              329
_journal_paper_doi               10.1039/b314192f
_journal_volume                  28
_journal_year                    2004
_chemical_formula_moiety         'C30 H18 O4.C4 H8 O2'
_chemical_formula_sum            'C34 H26 O6'
_chemical_formula_weight         530.55
_chemical_name_common
;2,3-bis-fluoren-9-ylidene-succinic acid ethyl acetate solvate
(1:1)
;
_chemical_name_systematic
;
2,3-bis-fluoren-9-ylidene-succinic acid ethyl acetate solvate (1:1)
;
_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'
_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                 94.282(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.1730(1)
_cell_length_b                   12.3379(2)
_cell_length_c                   17.7792(2)
_cell_measurement_reflns_used    12170
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      1.02
_cell_volume                     2662.79(6)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (2000)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius Kappa CCD diffractometer'
_diffrn_measurement_method
'COmbination of phi- and omega-scans,1.0 deg.'
_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  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0358
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12170
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         3.20
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  0.9821
_exptl_absorpt_correction_T_min  0.9821
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   -
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.240
_refine_diff_density_min         -0.232
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       -
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         6306
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0457P)²+0.4817P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.0978
_reflns_number_gt                4721
_reflns_number_total             6306
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b314192f.txt
_cod_data_source_block           c:\backup\xtal\tanaka\ta1etoac
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value '-' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7050252
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.19975(10) 0.37263(10) 0.62479(7) 0.0261(3) Uani 1 1 d . . .
H1 H 0.2740 0.3603 0.6409 0.031 Uiso 1 1 calc R . .
C2 C 0.14257(11) 0.29961(11) 0.57720(7) 0.0347(3) Uani 1 1 d . . .
H2 H 0.1787 0.2374 0.5612 0.042 Uiso 1 1 calc R . .
C3 C 0.03325(12) 0.31674(12) 0.55291(8) 0.0412(3) Uani 1 1 d . . .
H3 H -0.0040 0.2659 0.5210 0.049 Uiso 1 1 calc R . .
C4 C -0.02159(12) 0.40790(12) 0.57521(8) 0.0378(3) Uani 1 1 d . . .
H4 H -0.0957 0.4198 0.5586 0.045 Uiso 1 1 calc R . .
C5 C -0.10516(11) 0.63345(11) 0.64440(8) 0.0356(3) Uani 1 1 d . . .
H5 H -0.1634 0.6008 0.6149 0.043 Uiso 1 1 calc R . .
C6 C -0.11980(11) 0.73172(12) 0.67961(8) 0.0379(3) Uani 1 1 d . . .
H6 H -0.1889 0.7661 0.6746 0.045 Uiso 1 1 calc R . .
C7 C -0.03336(12) 0.77989(11) 0.72228(8) 0.0372(3) Uani 1 1 d . . .
H7 H -0.0444 0.8473 0.7451 0.045 Uiso 1 1 calc R . .
C8 C 0.06943(11) 0.73075(10) 0.73211(7) 0.0311(3) Uani 1 1 d . . .
H8 H 0.1274 0.7642 0.7613 0.037 Uiso 1 1 calc R . .
C9 C 0.18169(9) 0.55667(9) 0.69867(6) 0.0196(2) Uani 1 1 d . . .
C10 C 0.14527(9) 0.46454(9) 0.64841(6) 0.0207(2) Uani 1 1 d . . .
C11 C 0.03482(10) 0.48139(10) 0.62258(7) 0.0257(3) Uani 1 1 d . . .
C12 C -0.00266(10) 0.58399(10) 0.65349(7) 0.0257(3) Uani 1 1 d . . .
C13 C 0.08498(10) 0.63101(9) 0.69789(6) 0.0226(2) Uani 1 1 d . . .
C14 C 0.28026(9) 0.56858(9) 0.73756(6) 0.0188(2) Uani 1 1 d . . .
C15 C 0.37297(9) 0.48883(9) 0.73283(6) 0.0220(2) Uani 1 1 d . . .
O16 O 0.45138(7) 0.50728(7) 0.69768(5) 0.0363(2) Uani 1 1 d . . .
O17 O 0.36069(8) 0.39960(7) 0.77300(5) 0.0317(2) Uani 1 1 d . . .
H17 H 0.4204(17) 0.3514(17) 0.7664(11) 0.078(6) Uiso 1 1 d . . .
C18 C 0.31526(9) 0.66546(9) 0.78379(6) 0.0198(2) Uani 1 1 d . . .
C19 C 0.38332(10) 0.74516(9) 0.74275(6) 0.0218(2) Uani 1 1 d . . .
O20 O 0.48253(7) 0.75119(7) 0.75296(5) 0.0328(2) Uani 1 1 d . . .
O21 O 0.32331(8) 0.80567(8) 0.69483(5) 0.0374(2) Uani 1 1 d . . .
H21 H 0.3671(16) 0.8612(16) 0.6689(10) 0.074(6) Uiso 1 1 d . . .
C22 C 0.36677(10) 0.87918(10) 0.88421(7) 0.0277(3) Uani 1 1 d . . .
H22 H 0.3919 0.8905 0.8361 0.033 Uiso 1 1 calc R . .
C23 C 0.37779(11) 0.95984(11) 0.93869(7) 0.0323(3) Uani 1 1 d . . .
H23 H 0.4106 1.0262 0.9272 0.039 Uiso 1 1 calc R . .
C24 C 0.34113(12) 0.94383(11) 1.00968(7) 0.0352(3) Uani 1 1 d . . .
H24 H 0.3501 0.9991 1.0460 0.042 Uiso 1 1 calc R . .
C25 C 0.29134(11) 0.84728(11) 1.02770(7) 0.0316(3) Uani 1 1 d . . .
H25 H 0.2660 0.8368 1.0758 0.038 Uiso 1 1 calc R . .
C26 C 0.17822(10) 0.60806(11) 1.03437(7) 0.0296(3) Uani 1 1 d . . .
H26 H 0.1734 0.6427 1.0811 0.036 Uiso 1 1 calc R . .
C27 C 0.13560(11) 0.50505(11) 1.02217(7) 0.0327(3) Uani 1 1 d . . .
H27 H 0.1018 0.4693 1.0610 0.039 Uiso 1 1 calc R . .
C28 C 0.14222(11) 0.45400(11) 0.95314(7) 0.0319(3) Uani 1 1 d . . .
H28 H 0.1131 0.3839 0.9459 0.038 Uiso 1 1 calc R . .
C29 C 0.19114(10) 0.50488(10) 0.89452(7) 0.0277(3) Uani 1 1 d . . .
H29 H 0.1948 0.4699 0.8478 0.033 Uiso 1 1 calc R . .
C30 C 0.29306(9) 0.68215(9) 0.85598(6) 0.0208(2) Uani 1 1 d . . .
C31 C 0.31817(9) 0.78156(9) 0.90171(6) 0.0224(2) Uani 1 1 d . . .
C32 C 0.27949(10) 0.76637(10) 0.97353(6) 0.0240(3) Uani 1 1 d . . .
C33 C 0.22824(9) 0.65938(10) 0.97631(6) 0.0238(3) Uani 1 1 d . . .
C34 C 0.23462(9) 0.60823(9) 0.90588(6) 0.0224(2) Uani 1 1 d . . .
C35 C 0.41762(14) 1.22608(13) 0.47788(9) 0.0488(4) Uani 1 1 d . . .
H35B H 0.4469 1.2874 0.5071 0.073 Uiso 1 1 calc R . .
H35C H 0.3400 1.2377 0.4639 0.073 Uiso 1 1 calc R . .
H35A H 0.4569 1.2186 0.4327 0.073 Uiso 1 1 calc R . .
C36 C 0.43171(12) 1.12488(11) 0.52421(8) 0.0372(3) Uani 1 1 d . . .
H36A H 0.4008 1.0626 0.4958 0.045 Uiso 1 1 calc R . .
H36B H 0.5101 1.1111 0.5374 0.045 Uiso 1 1 calc R . .
O37 O 0.37409(8) 1.14111(7) 0.59206(5) 0.0355(2) Uani 1 1 d . . .
C38 C 0.36910(11) 1.05769(11) 0.63857(7) 0.0328(3) Uani 1 1 d . . .
O39 O 0.41293(8) 0.97094(8) 0.62746(5) 0.0381(2) Uani 1 1 d . . .
C40 C 0.30457(13) 1.08228(13) 0.70432(8) 0.0461(4) Uani 1 1 d . . .
H40A H 0.2780 1.1564 0.7007 0.069 Uiso 0.50 1 calc PR . .
H40B H 0.3512 1.0734 0.7506 0.069 Uiso 0.50 1 calc PR . .
H40C H 0.2424 1.0331 0.7045 0.069 Uiso 0.50 1 calc PR . .
H40D H 0.3031 1.0189 0.7365 0.069 Uiso 0.50 1 calc PR . .
H40E H 0.2299 1.1018 0.6866 0.069 Uiso 0.50 1 calc PR . .
H40F H 0.3387 1.1422 0.7327 0.069 Uiso 0.50 1 calc PR . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C10 118.93(12) . . ?
C3 C2 C1 121.20(12) . . ?
C4 C3 C2 120.58(12) . . ?
C3 C4 C11 118.66(13) . . ?
C6 C5 C12 118.57(12) . . ?
C5 C6 C7 120.42(12) . . ?
C6 C7 C8 121.47(13) . . ?
C7 C8 C13 118.77(12) . . ?
C14 C9 C13 127.57(10) . . ?
C14 C9 C10 127.12(10) . . ?
C13 C9 C10 105.29(9) . . ?
C1 C10 C11 119.18(11) . . ?
C1 C10 C9 132.30(11) . . ?
C11 C10 C9 108.52(10) . . ?
C4 C11 C10 121.44(12) . . ?
C4 C11 C12 129.75(12) . . ?
C10 C11 C12 108.81(10) . . ?
C5 C12 C13 121.51(12) . . ?
C5 C12 C11 129.66(12) . . ?
C13 C12 C11 108.83(10) . . ?
C8 C13 C12 119.24(11) . . ?
C8 C13 C9 132.26(11) . . ?
C12 C13 C9 108.49(10) . . ?
C9 C14 C18 125.15(10) . . ?
C9 C14 C15 122.89(10) . . ?
C18 C14 C15 111.69(9) . . ?
O16 C15 O17 124.28(11) . . ?
O16 C15 C14 122.26(11) . . ?
O17 C15 C14 113.42(10) . . ?
C30 C18 C14 125.24(10) . . ?
C30 C18 C19 121.18(10) . . ?
C14 C18 C19 113.56(9) . . ?
O20 C19 O21 124.27(11) . . ?
O20 C19 C18 123.06(10) . . ?
O21 C19 C18 112.67(10) . . ?
C31 C22 C23 119.10(11) . . ?
C24 C23 C22 120.87(12) . . ?
C23 C24 C25 120.68(12) . . ?
C24 C25 C32 118.88(11) . . ?
C27 C26 C33 118.82(11) . . ?
C26 C27 C28 120.66(12) . . ?
C27 C28 C29 121.01(12) . . ?
C28 C29 C34 119.07(11) . . ?
C18 C30 C34 127.78(10) . . ?
C18 C30 C31 126.73(10) . . ?
C34 C30 C31 105.45(9) . . ?
C22 C31 C32 119.78(11) . . ?
C22 C31 C30 131.72(10) . . ?
C32 C31 C30 108.47(10) . . ?
C25 C32 C31 120.67(11) . . ?
C25 C32 C33 130.44(11) . . ?
C31 C32 C33 108.88(10) . . ?
C26 C33 C34 120.81(11) . . ?
C26 C33 C32 130.40(11) . . ?
C34 C33 C32 108.80(10) . . ?
C29 C34 C33 119.62(11) . . ?
C29 C34 C30 131.98(10) . . ?
C33 C34 C30 108.39(10) . . ?
O37 C36 C35 107.39(12) . . ?
C38 O37 C36 117.28(10) . . ?
O39 C38 O37 122.71(12) . . ?
O39 C38 C40 124.73(13) . . ?
O37 C38 C40 112.56(12) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.3871(17) . ?
C1 C10 1.3942(16) . ?
C2 C3 1.384(2) . ?
C3 C4 1.381(2) . ?
C4 C11 1.3844(18) . ?
C5 C6 1.382(2) . ?
C5 C12 1.3876(17) . ?
C6 C7 1.384(2) . ?
C7 C8 1.3897(18) . ?
C8 C13 1.3920(17) . ?
C9 C14 1.3475(16) . ?
C9 C13 1.4915(16) . ?
C9 C10 1.4926(15) . ?
C10 C11 1.4034(16) . ?
C11 C12 1.4663(17) . ?
C12 C13 1.4042(17) . ?
C14 C18 1.4945(15) . ?
C14 C15 1.5043(16) . ?
C15 O16 1.2010(14) . ?
C15 O17 1.3269(14) . ?
C18 C30 1.3470(16) . ?
C18 C19 1.5086(16) . ?
C19 O20 1.2101(14) . ?
C19 O21 1.3129(14) . ?
C22 C31 1.3874(17) . ?
C22 C23 1.3883(17) . ?
C23 C24 1.3839(19) . ?
C24 C25 1.385(2) . ?
C25 C32 1.3871(17) . ?
C26 C27 1.384(2) . ?
C26 C33 1.3896(17) . ?
C27 C28 1.3871(19) . ?
C28 C29 1.3884(17) . ?
C29 C34 1.3896(17) . ?
C30 C34 1.4898(16) . ?
C30 C31 1.4905(16) . ?
C31 C32 1.4062(16) . ?
C32 C33 1.4624(17) . ?
C33 C34 1.4095(16) . ?
C35 C36 1.499(2) . ?
C36 O37 1.4538(16) . ?
O37 C38 1.3245(15) . ?
C38 O39 1.2186(16) . ?
C38 C40 1.488(2) . ?
