#------------------------------------------------------------------------------
#$Date: 2017-10-14 22:27:35 +0300 (Sat, 14 Oct 2017) $
#$Revision: 202017 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/02/7050250.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_7050250
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.C3 H6 O'
_chemical_formula_sum            'C33 H24 O5'
_chemical_formula_weight         500.55
_chemical_name_common
'2,3-bis-fluoren-9-ylidene-succinic acid acetone solvate (1:1)'
_chemical_name_systematic
;
2,3-bis-fluoren-9-ylidene-succinic acid acetone solvate (1:1)
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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            4
_cell_length_a                   9.9117(2)
_cell_length_b                   14.1651(3)
_cell_length_c                   18.1568(5)
_cell_measurement_reflns_used    11267
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      27.10
_cell_measurement_theta_min      1.02
_cell_volume                     2549.22(10)
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'phi- and omega-scans of 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  0.040
_diffrn_reflns_av_sigmaI/netI    0.0702
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11267
_diffrn_reflns_theta_full        27.11
_diffrn_reflns_theta_max         27.11
_diffrn_reflns_theta_min         3.66
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  0.9896
_exptl_absorpt_correction_T_min  0.9827
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   -
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.523
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.4(14)
_refine_ls_extinction_coef       -
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         5507
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0944
_refine_ls_R_factor_gt           0.0545
_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)+(0.0723P)²+0.3252P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1220
_refine_ls_wR_factor_ref         0.1392
_reflns_number_gt                3816
_reflns_number_total             5507
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b314192f.txt
_cod_data_source_block           a:\tanak2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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)2(1)2(1)
_cod_database_code               7050250
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -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 0.3628(3) 0.59506(18) 0.57951(16) 0.0377(7) Uani 1 1 d . . .
H1 H 0.3645 0.6209 0.5318 0.045 Uiso 1 1 calc R . .
C2 C 0.2496(3) 0.6041(2) 0.62287(19) 0.0524(9) Uani 1 1 d . . .
H2 H 0.1739 0.6363 0.6045 0.063 Uiso 1 1 calc R . .
C3 C 0.2457(3) 0.5663(3) 0.69339(19) 0.0579(9) Uani 1 1 d . . .
H3 H 0.1673 0.5728 0.7221 0.069 Uiso 1 1 calc R . .
C4 C 0.3558(3) 0.5194(2) 0.72140(17) 0.0453(8) Uani 1 1 d . . .
H4 H 0.3538 0.4945 0.7694 0.054 Uiso 1 1 calc R . .
C5 C 0.6396(3) 0.41580(19) 0.75711(15) 0.0392(7) Uani 1 1 d . . .
H5 H 0.5823 0.4110 0.7982 0.047 Uiso 1 1 calc R . .
C6 C 0.7670(3) 0.3759(2) 0.75819(16) 0.0434(8) Uani 1 1 d . . .
H6 H 0.7963 0.3425 0.8000 0.052 Uiso 1 1 calc R . .
C7 C 0.8511(3) 0.3850(2) 0.69809(16) 0.0409(7) Uani 1 1 d . . .
H7 H 0.9378 0.3583 0.7000 0.049 Uiso 1 1 calc R . .
C8 C 0.8113(3) 0.43244(19) 0.63490(15) 0.0335(6) Uani 1 1 d . . .
H8 H 0.8704 0.4384 0.5947 0.040 Uiso 1 1 calc R . .
C9 C 0.6089(3) 0.52582(15) 0.57448(13) 0.0245(5) Uani 1 1 d . . .
C10 C 0.4744(2) 0.54744(16) 0.60685(14) 0.0274(6) Uani 1 1 d . . .
C11 C 0.4691(3) 0.50955(17) 0.67822(15) 0.0303(6) Uani 1 1 d . . .
C12 C 0.5981(3) 0.46318(17) 0.69407(14) 0.0298(6) Uani 1 1 d . . .
C13 C 0.6819(3) 0.47118(17) 0.63220(14) 0.0279(6) Uani 1 1 d . . .
C14 C 0.6555(3) 0.55311(16) 0.50809(14) 0.0261(6) Uani 1 1 d . . .
C15 C 0.5781(3) 0.61839(18) 0.45935(15) 0.0293(6) Uani 1 1 d . . .
O16 O 0.5856(2) 0.70315(13) 0.46501(11) 0.0435(5) Uani 1 1 d . . .
O17 O 0.5075(2) 0.57505(14) 0.40841(11) 0.0460(5) Uani 1 1 d . . .
H17 H 0.4665 0.6146 0.3832 0.055 Uiso 1 1 calc R . .
C18 C 0.7945(3) 0.53462(16) 0.47915(13) 0.0248(5) Uani 1 1 d . . .
C19 C 0.8812(3) 0.62182(17) 0.47923(15) 0.0290(6) Uani 1 1 d . . .
O20 O 0.9144(2) 0.66364(13) 0.42518(11) 0.0477(5) Uani 1 1 d . . .
O21 O 0.9125(2) 0.64890(14) 0.54718(10) 0.0428(5) Uani 1 1 d . . .
H21 H 0.9523 0.7004 0.5456 0.051 Uiso 1 1 calc R . .
C22 C 1.0991(3) 0.48001(19) 0.43496(16) 0.0362(6) Uani 1 1 d . . .
H22 H 1.0990 0.5420 0.4533 0.043 Uiso 1 1 calc R . .
C23 C 1.2193(3) 0.4371(2) 0.41336(17) 0.0429(7) Uani 1 1 d . . .
H23 H 1.3009 0.4704 0.4178 0.051 Uiso 1 1 calc R . .
C24 C 1.2204(3) 0.3463(2) 0.38542(17) 0.0445(7) Uani 1 1 d . . .
H24 H 1.3022 0.3194 0.3698 0.053 Uiso 1 1 calc R . .
C25 C 1.1036(3) 0.29506(19) 0.38031(16) 0.0401(7) Uani 1 1 d . . .
H25 H 1.1048 0.2331 0.3618 0.048 Uiso 1 1 calc R . .
C26 C 0.8037(3) 0.20502(18) 0.39431(17) 0.0396(7) Uani 1 1 d . . .
H26 H 0.8634 0.1592 0.3759 0.048 Uiso 1 1 calc R . .
C27 C 0.6692(3) 0.18339(18) 0.40596(16) 0.0421(7) Uani 1 1 d . . .
H27 H 0.6374 0.1222 0.3959 0.051 Uiso 1 1 calc R . .
C28 C 0.5816(3) 0.25114(18) 0.43231(15) 0.0376(7) Uani 1 1 d . . .
H28 H 0.4902 0.2357 0.4390 0.045 Uiso 1 1 calc R . .
C29 C 0.6257(3) 0.34133(18) 0.44907(14) 0.0313(6) Uani 1 1 d . . .
H29 H 0.5651 0.3866 0.4674 0.038 Uiso 1 1 calc R . .
C30 C 0.8387(3) 0.45273(16) 0.45103(13) 0.0250(6) Uani 1 1 d . . .
C31 C 0.9812(2) 0.43018(17) 0.42891(14) 0.0267(6) Uani 1 1 d . . .
C32 C 0.9833(3) 0.33624(17) 0.40302(14) 0.0311(6) Uani 1 1 d . . .
C33 C 0.8487(3) 0.29531(16) 0.41017(14) 0.0303(6) Uani 1 1 d . . .
C34 C 0.7609(3) 0.36409(16) 0.43838(13) 0.0266(6) Uani 1 1 d . . .
C35 C 0.3172(4) 0.7542(2) 0.30325(17) 0.0531(9) Uani 1 1 d . . .
C36 C 0.3528(5) 0.8390(3) 0.2613(2) 0.0858(14) Uani 1 1 d . . .
H36A H 0.3575 0.8927 0.2943 0.129 Uiso 1 1 calc R . .
H36B H 0.2848 0.8505 0.2240 0.129 Uiso 1 1 calc R . .
H36C H 0.4398 0.8299 0.2379 0.129 Uiso 1 1 calc R . .
C37 C 0.1788(5) 0.7426(4) 0.3248(4) 0.130(2) Uani 1 1 d . . .
H37A H 0.1639 0.6780 0.3405 0.195 Uiso 1 1 calc R . .
H37B H 0.1206 0.7568 0.2833 0.195 Uiso 1 1 calc R . .
H37C H 0.1585 0.7852 0.3651 0.195 Uiso 1 1 calc R . .
O38 O 0.4089(4) 0.7010(3) 0.31745(15) 0.1285(16) Uani 1 1 d . . .
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 119.4(3) . . ?
C1 C2 C3 121.0(3) . . ?
C4 C3 C2 120.3(3) . . ?
C3 C4 C11 119.1(3) . . ?
C6 C5 C12 118.6(3) . . ?
C7 C6 C5 120.1(3) . . ?
C6 C7 C8 121.9(3) . . ?
C7 C8 C13 118.7(3) . . ?
C14 C9 C10 126.9(2) . . ?
C14 C9 C13 127.7(2) . . ?
C10 C9 C13 105.3(2) . . ?
C1 C10 C11 119.1(2) . . ?
C1 C10 C9 132.3(2) . . ?
C11 C10 C9 108.6(2) . . ?
C4 C11 C10 121.2(3) . . ?
C4 C11 C12 130.2(3) . . ?
C10 C11 C12 108.6(2) . . ?
C5 C12 C13 121.6(3) . . ?
C5 C12 C11 129.5(3) . . ?
C13 C12 C11 108.9(2) . . ?
C8 C13 C12 119.0(2) . . ?
C8 C13 C9 132.5(2) . . ?
C12 C13 C9 108.5(2) . . ?
C9 C14 C15 122.1(2) . . ?
C9 C14 C18 125.4(2) . . ?
C15 C14 C18 111.9(2) . . ?
O16 C15 O17 123.9(2) . . ?
O16 C15 C14 122.3(2) . . ?
O17 C15 C14 113.7(2) . . ?
C30 C18 C14 125.9(2) . . ?
C30 C18 C19 121.6(2) . . ?
C14 C18 C19 112.4(2) . . ?
O20 C19 O21 123.8(2) . . ?
O20 C19 C18 124.4(2) . . ?
O21 C19 C18 111.8(2) . . ?
C31 C22 C23 118.8(2) . . ?
C24 C23 C22 121.0(3) . . ?
C25 C24 C23 120.8(3) . . ?
C24 C25 C32 118.9(3) . . ?
C27 C26 C33 118.9(3) . . ?
C28 C27 C26 120.3(2) . . ?
C27 C28 C29 121.3(3) . . ?
C28 C29 C34 119.1(2) . . ?
C18 C30 C34 128.1(2) . . ?
C18 C30 C31 126.4(2) . . ?
C34 C30 C31 105.4(2) . . ?
C22 C31 C32 120.0(2) . . ?
C22 C31 C30 132.1(2) . . ?
C32 C31 C30 107.6(2) . . ?
C25 C32 C31 120.5(2) . . ?
C25 C32 C33 130.0(2) . . ?
C31 C32 C33 109.4(2) . . ?
C26 C33 C34 121.1(3) . . ?
C26 C33 C32 130.0(2) . . ?
C34 C33 C32 108.9(2) . . ?
C29 C34 C33 119.2(2) . . ?
C29 C34 C30 132.2(2) . . ?
C33 C34 C30 108.6(2) . . ?
O38 C35 C37 126.2(5) . . ?
O38 C35 C36 116.1(4) . . ?
C37 C35 C36 117.7(4) . . ?
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 1.377(4) . ?
C1 C10 1.387(4) . ?
C2 C3 1.388(5) . ?
C3 C4 1.375(5) . ?
C4 C11 1.376(4) . ?
C5 C6 1.384(4) . ?
C5 C12 1.389(4) . ?
C6 C7 1.379(4) . ?
C7 C8 1.387(4) . ?
C8 C13 1.396(4) . ?
C9 C14 1.348(3) . ?
C9 C10 1.489(4) . ?
C9 C13 1.490(4) . ?
C10 C11 1.404(4) . ?
C11 C12 1.466(4) . ?
C12 C13 1.402(4) . ?
C14 C15 1.492(4) . ?
C14 C18 1.497(4) . ?
C15 O16 1.207(3) . ?
C15 O17 1.312(3) . ?
C18 C30 1.341(3) . ?
C18 C19 1.505(3) . ?
C19 O20 1.192(3) . ?
C19 O21 1.329(3) . ?
C22 C31 1.370(4) . ?
C22 C23 1.394(4) . ?
C23 C24 1.383(4) . ?
C24 C25 1.369(4) . ?
C25 C32 1.390(4) . ?
C26 C27 1.384(4) . ?
C26 C33 1.385(4) . ?
C27 C28 1.379(4) . ?
C28 C29 1.384(4) . ?
C29 C34 1.392(4) . ?
C30 C34 1.492(3) . ?
C30 C31 1.503(3) . ?
C31 C32 1.411(3) . ?
C32 C33 1.460(4) . ?
C33 C34 1.404(3) . ?
C35 O38 1.209(4) . ?
C35 C37 1.435(5) . ?
C35 C36 1.466(5) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 21141940
