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#$Date: 2016-03-23 00:41:36 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179123 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/85/4308534.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_4308534
loop_
_publ_author_name
'Diane A. Dickie'
'Michael C. Jennings'
'Hilary A. Jenkins'
'Jason A. C. Clyburne'
_publ_contact_author_address
;Department of Chemistry
Simon Fraser University
8888 University Dr
Burnaby, BC V5A 1S6
Canada
;
_publ_contact_author_email       clyburne@sfu.ca
_publ_contact_author_fax         (604)291-3765
_publ_contact_author_name        'Jason Clyburne'
_publ_contact_author_phone       (604)291-4885
_publ_section_title
;
A Zinc Carboxylate Network Containing Metal Sites with Low Coordination
Numbers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              828
_journal_page_last               830
_journal_paper_doi               10.1021/ic048443h
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C20 H14 O4'
_chemical_formula_weight         318.31
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_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            8
_cell_length_a                   13.5640(3)
_cell_length_b                   13.5640(3)
_cell_length_c                   17.0150(4)
_cell_measurement_temperature    173(2)
_cell_volume                     3130.46(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0338
_diffrn_reflns_av_sigmaI/netI    0.0467
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6119
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.57
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  0.9906
_exptl_absorpt_correction_T_min  0.9814
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.194
_refine_diff_density_min         -0.128
_refine_diff_density_rms         0.032
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   1.0(12)
_refine_ls_extinction_coef       0.0024(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         3074
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0396
_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)+(0.0370P)²+0.4022P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0808
_refine_ls_wR_factor_ref         0.0885
_reflns_number_gt                2491
_reflns_number_total             3074
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048443hsi20041105_044950.cif
_cod_data_source_block           sask1
_cod_database_code               4308534
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, -z+3/4'
'-x+1/2, y+1/2, -z+1/4'
'-y, -x, -z+1/2'
'y, x, -z'
'y+1/2, -x+1/2, z+3/4'
'-y+1/2, x+1/2, z+1/4'
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
O1 O 0.21747(9) 0.33338(10) -0.50290(9) 0.0417(4) Uani 1 1 d . . .
H1 H 0.1809 0.2834 -0.5026 0.063 Uiso 0.50 1 calc PR . .
O2 O 0.66595(9) 0.60956(9) -0.44241(8) 0.0355(3) Uani 1 1 d . . .
H2 H 0.7063 0.6559 -0.4486 0.053 Uiso 0.50 1 calc PR . .
O3 O 0.41832(10) 0.69417(9) -0.23335(9) 0.0418(4) Uani 1 1 d . . .
H3 H 0.3686 0.7310 -0.2353 0.063 Uiso 0.50 1 calc PR . .
O4 O 0.68897(10) 0.23874(9) -0.30132(8) 0.0382(4) Uani 1 1 d . . .
H4 H 0.7363 0.1994 -0.2957 0.057 Uiso 0.50 1 calc PR . .
C1 C 0.30670(12) 0.30670(12) -0.5000 0.0290(6) Uani 1 2 d S . .
C2 C 0.38422(13) 0.38422(13) -0.5000 0.0281(6) Uani 1 2 d S . .
C3 C 0.48288(13) 0.35825(13) -0.50880(11) 0.0306(4) Uani 1 1 d . . .
H3A H 0.5002 0.2908 -0.5144 0.037 Uiso 1 1 calc R . .
C4 C 0.55676(13) 0.42996(13) -0.50948(11) 0.0285(4) Uani 1 1 d . . .
C5 C 0.52910(12) 0.52910(12) -0.5000 0.0270(6) Uani 1 2 d S . .
C6 C 0.60721(12) 0.60721(12) -0.5000 0.0265(6) Uani 1 2 d S . .
C7 C 0.66158(13) 0.40025(13) -0.51997(11) 0.0294(4) Uani 1 1 d . . .
C8 C 0.72265(15) 0.44604(15) -0.57462(13) 0.0387(5) Uani 1 1 d . . .
H8A H 0.6972 0.4965 -0.6076 0.046 Uiso 1 1 calc R . .
C9 C 0.82061(16) 0.41800(17) -0.58089(15) 0.0521(6) Uani 1 1 d . . .
H9A H 0.8619 0.4490 -0.6186 0.062 Uiso 1 1 calc R . .
C10 C 0.85864(16) 0.34546(18) -0.53281(16) 0.0536(7) Uani 1 1 d . . .
H10A H 0.9261 0.3273 -0.5368 0.064 Uiso 1 1 calc R . .
C11 C 0.79870(15) 0.29988(16) -0.47927(14) 0.0453(6) Uani 1 1 d . . .
H11A H 0.8248 0.2500 -0.4460 0.054 Uiso 1 1 calc R . .
C12 C 0.70027(14) 0.32599(14) -0.47328(12) 0.0354(5) Uani 1 1 d . . .
H12A H 0.6589 0.2927 -0.4369 0.042 Uiso 1 1 calc R . .
C13 C 0.39333(12) 0.60667(12) -0.2500 0.0294(6) Uani 1 2 d S . .
C14 C 0.47125(12) 0.52875(12) -0.2500 0.0288(6) Uani 1 2 d S . .
C15 C 0.56952(13) 0.55505(13) -0.24295(11) 0.0302(4) Uani 1 1 d . . .
H15A H 0.5867 0.6225 -0.2364 0.036 Uiso 1 1 calc R . .
C16 C 0.64363(12) 0.48381(13) -0.24541(11) 0.0276(4) Uani 1 1 d . . .
C17 C 0.61628(12) 0.38372(12) -0.2500 0.0263(6) Uani 1 2 d S . .
C18 C 0.69436(12) 0.30564(12) -0.2500 0.0250(6) Uani 1 2 d S . .
C19 C 0.74842(13) 0.51670(13) -0.24800(12) 0.0278(4) Uani 1 1 d . . .
C20 C 0.80476(14) 0.49773(14) -0.31418(12) 0.0376(5) Uani 1 1 d . . .
H20A H 0.7776 0.4612 -0.3566 0.045 Uiso 1 1 calc R . .
C21 C 0.90106(15) 0.53215(15) -0.31854(15) 0.0447(6) Uani 1 1 d . . .
H21A H 0.9392 0.5197 -0.3643 0.054 Uiso 1 1 calc R . .
C22 C 0.94159(15) 0.58395(15) -0.25732(14) 0.0433(6) Uani 1 1 d . . .
H22A H 1.0078 0.6064 -0.2605 0.052 Uiso 1 1 calc R . .
C23 C 0.88644(15) 0.60328(15) -0.19157(13) 0.0423(5) Uani 1 1 d . . .
H23A H 0.9144 0.6394 -0.1492 0.051 Uiso 1 1 calc R . .
C24 C 0.78946(15) 0.56995(14) -0.18684(12) 0.0361(5) Uani 1 1 d . . .
H24A H 0.7513 0.5839 -0.1414 0.043 Uiso 1 1 calc R . .
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
C1 O1 H1 109.5 . . ?
C6 O2 H2 109.5 . . ?
C13 O3 H3 109.5 . . ?
C18 O4 H4 109.5 . . ?
O1 C1 O1 123.3(2) 6_554 . ?
O1 C1 C2 118.33(11) 6_554 . ?
O1 C1 C2 118.33(11) . . ?
C3 C2 C3 119.9(2) 6_554 . ?
C3 C2 C1 120.06(11) 6_554 . ?
C3 C2 C1 120.06(11) . . ?
C2 C3 C4 120.96(17) . . ?
C2 C3 H3A 119.5 . . ?
C4 C3 H3A 119.5 . . ?
C3 C4 C5 118.29(17) . . ?
C3 C4 C7 119.85(16) . . ?
C5 C4 C7 121.85(16) . . ?
C4 C5 C4 121.6(2) 6_554 . ?
C4 C5 C6 119.20(11) 6_554 . ?
C4 C5 C6 119.20(11) . . ?
O2 C6 O2 124.7(2) . 6_554 ?
O2 C6 C5 117.63(11) . . ?
O2 C6 C5 117.63(11) 6_554 . ?
C12 C7 C8 118.82(17) . . ?
C12 C7 C4 119.32(16) . . ?
C8 C7 C4 121.85(18) . . ?
C9 C8 C7 120.0(2) . . ?
C9 C8 H8A 120.0 . . ?
C7 C8 H8A 120.0 . . ?
C10 C9 C8 120.6(2) . . ?
C10 C9 H9A 119.7 . . ?
C8 C9 H9A 119.7 . . ?
C11 C10 C9 119.6(2) . . ?
C11 C10 H10A 120.2 . . ?
C9 C10 H10A 120.2 . . ?
C10 C11 C12 120.4(2) . . ?
C10 C11 H11A 119.8 . . ?
C12 C11 H11A 119.8 . . ?
C11 C12 C7 120.6(2) . . ?
C11 C12 H12A 119.7 . . ?
C7 C12 H12A 119.7 . . ?
O3 C13 O3 123.5(2) 5_664 . ?
O3 C13 C14 118.25(11) 5_664 . ?
O3 C13 C14 118.25(11) . . ?
C15 C14 C15 120.2(2) 5_664 . ?
C15 C14 C13 119.89(11) 5_664 . ?
C15 C14 C13 119.89(11) . . ?
C14 C15 C16 120.83(17) . . ?
C14 C15 H15A 119.6 . . ?
C16 C15 H15A 119.6 . . ?
C15 C16 C17 118.64(16) . . ?
C15 C16 C19 118.74(15) . . ?
C17 C16 C19 122.52(15) . . ?
C16 C17 C16 120.7(2) . 5_664 ?
C16 C17 C18 119.67(11) . . ?
C16 C17 C18 119.67(11) 5_664 . ?
O4 C18 O4 124.2(2) 5_664 . ?
O4 C18 C17 117.88(11) 5_664 . ?
O4 C18 C17 117.88(11) . . ?
C24 C19 C20 119.11(17) . . ?
C24 C19 C16 121.17(17) . . ?
C20 C19 C16 119.66(18) . . ?
C19 C20 C21 120.0(2) . . ?
C19 C20 H20A 120.0 . . ?
C21 C20 H20A 120.0 . . ?
C22 C21 C20 120.6(2) . . ?
C22 C21 H21A 119.7 . . ?
C20 C21 H21A 119.7 . . ?
C23 C22 C21 119.93(19) . . ?
C23 C22 H22A 120.0 . . ?
C21 C22 H22A 120.0 . . ?
C22 C23 C24 120.0(2) . . ?
C22 C23 H23A 120.0 . . ?
C24 C23 H23A 120.0 . . ?
C19 C24 C23 120.38(19) . . ?
C19 C24 H24A 119.8 . . ?
C23 C24 H24A 119.8 . . ?
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
O1 C1 1.2642(16) . ?
O1 H1 0.8400 . ?
O2 C6 1.2633(16) . ?
O2 H2 0.8400 . ?
O3 C13 1.2663(17) . ?
O3 H3 0.8400 . ?
O4 C18 1.2614(16) . ?
O4 H4 0.8400 . ?
C1 O1 1.2642(16) 6_554 ?
C1 C2 1.487(3) . ?
C2 C3 1.392(2) 6_554 ?
C2 C3 1.392(2) . ?
C3 C4 1.397(3) . ?
C3 H3A 0.9500 . ?
C4 C5 1.405(2) . ?
C4 C7 1.489(2) . ?
C5 C4 1.405(2) 6_554 ?
C5 C6 1.498(3) . ?
C6 O2 1.2633(16) 6_554 ?
C7 C12 1.386(3) . ?
C7 C8 1.392(3) . ?
C8 C9 1.386(3) . ?
C8 H8A 0.9500 . ?
C9 C10 1.380(3) . ?
C9 H9A 0.9500 . ?
C10 C11 1.369(3) . ?
C10 H10A 0.9500 . ?
C11 C12 1.385(3) . ?
C11 H11A 0.9500 . ?
C12 H12A 0.9500 . ?
C13 O3 1.2663(17) 5_664 ?
C13 C14 1.495(3) . ?
C14 C15 1.385(2) 5_664 ?
C14 C15 1.385(2) . ?
C15 C16 1.395(3) . ?
C15 H15A 0.9500 . ?
C16 C17 1.410(2) . ?
C16 C19 1.490(2) . ?
C17 C16 1.410(2) 5_664 ?
C17 C18 1.498(3) . ?
C18 O4 1.2614(16) 5_664 ?
C19 C24 1.384(3) . ?
C19 C20 1.385(3) . ?
C20 C21 1.389(3) . ?
C20 H20A 0.9500 . ?
C21 C22 1.371(3) . ?
C21 H21A 0.9500 . ?
C22 C23 1.371(3) . ?
C22 H22A 0.9500 . ?
C23 C24 1.393(3) . ?
C23 H23A 0.9500 . ?
C24 H24A 0.9500 . ?
