#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/96/4329667.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_4329667
loop_
_publ_author_name
'Ya-Qian Lan'
'Hai-Long Jiang'
'Shun-Li Li'
'Qiang Xu'
_publ_section_title
;
 Solvent-Induced Controllable Synthesis, Single-Crystal to Single-Crystal
 Transformation and Encapsulation of Alq3 for Modulated Luminescence in
 (4,8)-Connected Metal-Organic Frameworks
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7484
_journal_page_last               7491
_journal_paper_doi               10.1021/ic202635a
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C37 H28 O24 Zn4'
_chemical_formula_weight         1118.07
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           130
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a 2ac'
_symmetry_space_group_name_H-M   'P 4/n c c :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            4
_cell_length_a                   19.0396(17)
_cell_length_b                   19.0396(17)
_cell_length_c                   23.563(2)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.03
_cell_volume                     8541.7(13)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'Diamond (Brandenburg and Putz, 2008)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97(Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0908
_diffrn_reflns_av_sigmaI/netI    0.0522
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            59363
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.03
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.155
_exptl_absorpt_correction_T_max  0.741
_exptl_absorpt_correction_T_min  0.714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.869
_exptl_crystal_description       block
_exptl_crystal_F_000             2248
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.26
_platon_squeeze_details          ' ?'
_refine_diff_density_max         0.576
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         4844
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.945
_refine_ls_R_factor_all          0.1016
_refine_ls_R_factor_gt           0.0707
_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)+(0.1461P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2075
_refine_ls_wR_factor_ref         0.2251
_reflns_number_gt                2777
_reflns_number_total             4844
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202635a_si_002_5.cif
_cod_data_source_block           1h2o
_cod_original_cell_volume        8541.6(13)
_cod_original_sg_symbol_Hall     '-P 4a 2ac '
_cod_original_sg_symbol_H-M      'P 4/n c c'
_cod_database_code               4329667
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'x+1/2, -y, -z+1/2'
'-x, y+1/2, -z+1/2'
'-y, -x, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'y, -x+1/2, z'
'-y+1/2, x, z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'-x-1/2, y, z-1/2'
'x, -y-1/2, z-1/2'
'y, x, z-1/2'
'-y-1/2, -x-1/2, z-1/2'
'-y, x-1/2, -z'
'y-1/2, -x, -z'
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
Zn1 Zn 0.47292(3) 0.45114(3) 0.703969(19) 0.0536(2) Uani 1 1 d .
O5 O 0.78007(14) 0.33965(18) 0.56550(12) 0.0757(9) Uani 1 1 d .
C3 C 0.7690(2) 0.3886(2) 0.60720(18) 0.0653(11) Uani 1 1 d .
C1 C 0.7500 0.2500 0.5000 0.0558(18) Uani 1 4 d S
C5 C 0.6994(2) 0.4536(2) 0.67363(17) 0.0642(11) Uani 1 1 d .
O1 O 0.57611(16) 0.44257(18) 0.67802(13) 0.0766(9) Uani 1 1 d .
C4 C 0.7034(2) 0.4066(2) 0.62810(17) 0.0658(11) Uani 1 1 d .
H6 H 0.6628 0.3877 0.6122 0.079 Uiso 1 1 calc R
C2 C 0.72181(19) 0.3092(2) 0.53751(16) 0.0572(10) Uani 1 1 d .
H9A H 0.6980 0.3441 0.5145 0.069 Uiso 1 1 calc R
H9B H 0.6887 0.2907 0.5650 0.069 Uiso 1 1 calc R
C6 C 0.7602(2) 0.4811(3) 0.69742(18) 0.0674(11) Uani 1 1 d .
H3 H 0.7572 0.5114 0.7283 0.081 Uiso 1 1 calc R
C8 C 0.8293(2) 0.4171(3) 0.63044(17) 0.0688(12) Uani 1 1 d .
H8 H 0.8730 0.4048 0.6157 0.083 Uiso 1 1 calc R
C7 C 0.8254(2) 0.4636(2) 0.67524(18) 0.0690(12) Uani 1 1 d .
O1W O 0.4277(2) 0.4051(2) 0.63830(16) 0.1090(13) Uani 1 1 d .
C9 C 0.6282(2) 0.4692(2) 0.70094(17) 0.0613(11) Uani 1 1 d .
O2 O 0.62959(16) 0.50913(18) 0.74284(12) 0.0778(9) Uani 1 1 d .
C10 C 0.8924(3) 0.4884(3) 0.70296(18) 0.0678(12) Uani 1 1 d .
O3 O 0.94839(17) 0.47332(19) 0.67855(15) 0.0840(10) Uani 1 1 d .
O4 O 0.88604(17) 0.52290(18) 0.74847(13) 0.0854(10) 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'
Zn Zn 0.2839 1.4301 '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
O1W Zn1 O3 100.99(17) . 7_565
O1W Zn1 O2 102.90(16) . 5_666
O3 Zn1 O2 156.11(14) 7_565 5_666
O1W Zn1 O4 100.51(16) . 3_466
O3 Zn1 O4 86.36(15) 7_565 3_466
O2 Zn1 O4 88.90(15) 5_666 3_466
O1W Zn1 O1 98.51(15) . .
O3 Zn1 O1 89.04(14) 7_565 .
O2 Zn1 O1 87.85(14) 5_666 .
O4 Zn1 O1 160.95(13) 3_466 .
O1W Zn1 Zn1 175.13(15) . 5_666
O3 Zn1 Zn1 75.68(10) 7_565 5_666
O2 Zn1 Zn1 80.50(9) 5_666 5_666
O4 Zn1 Zn1 82.94(9) 3_466 5_666
O1 Zn1 Zn1 78.01(9) . 5_666
C3 O5 C2 119.5(3) . .
O5 C3 C4 124.1(4) . .
O5 C3 C8 114.9(4) . .
C4 C3 C8 120.8(4) . .
C2 C1 C2 109.51(16) 15_656 .
C2 C1 C2 109.4(3) 15_656 16_666
C2 C1 C2 109.51(16) . 16_666
C2 C1 C2 109.51(16) 15_656 2_655
C2 C1 C2 109.4(3) . 2_655
C2 C1 C2 109.51(16) 16_666 2_655
C6 C5 C4 120.4(4) . .
C6 C5 C9 119.8(4) . .
C4 C5 C9 119.6(4) . .
C9 O1 Zn1 127.0(3) . .
C3 C4 C5 118.6(4) . .
C3 C4 H6 120.7 . .
C5 C4 H6 120.7 . .
O5 C2 C1 107.2(3) . .
O5 C2 H9A 110.3 . .
C1 C2 H9A 110.3 . .
O5 C2 H9B 110.3 . .
C1 C2 H9B 110.3 . .
H9A C2 H9B 108.5 . .
C5 C6 C7 120.2(4) . .
C5 C6 H3 119.9 . .
C7 C6 H3 119.9 . .
C7 C8 C3 120.6(4) . .
C7 C8 H8 119.7 . .
C3 C8 H8 119.7 . .
C8 C7 C6 119.4(4) . .
C8 C7 C10 119.1(4) . .
C6 C7 C10 121.2(4) . .
O1 C9 O2 127.8(4) . .
O1 C9 C5 116.6(4) . .
O2 C9 C5 115.6(4) . .
C9 O2 Zn1 125.5(3) . 5_666
O3 C10 O4 126.5(4) . .
O3 C10 C7 116.8(4) . .
O4 C10 C7 116.7(4) . .
C10 O3 Zn1 132.8(3) . 8_655
C10 O4 Zn1 120.7(3) . 3_566
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O1W 1.976(3) .
Zn1 O3 2.004(3) 7_565
Zn1 O2 2.012(3) 5_666
Zn1 O4 2.058(3) 3_466
Zn1 O1 2.064(3) .
Zn1 Zn1 2.9810(9) 5_666
O5 C3 1.371(5) .
O5 C2 1.415(5) .
C3 C4 1.385(6) .
C3 C8 1.384(6) .
C1 C2 1.530(4) 15_656
C1 C2 1.530(4) .
C1 C2 1.530(4) 16_666
C1 C2 1.530(4) 2_655
C5 C6 1.387(6) .
C5 C4 1.400(5) .
C5 C9 1.530(6) .
O1 C9 1.237(5) .
C4 H6 0.9300 .
C2 H9A 0.9700 .
C2 H9B 0.9700 .
C6 C7 1.389(6) .
C6 H3 0.9300 .
C8 C7 1.380(6) .
C8 H8 0.9300 .
C7 C10 1.509(6) .
C9 O2 1.247(4) .
O2 Zn1 2.012(3) 5_666
C10 O3 1.245(6) .
C10 O4 1.263(5) .
O3 Zn1 2.004(3) 8_655
O4 Zn1 2.058(3) 3_566
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C2 O5 C3 C4 6.2(7) . .
C2 O5 C3 C8 -177.7(4) . .
O1W Zn1 O1 C9 172.5(4) . .
O3 Zn1 O1 C9 71.5(4) 7_565 .
O2 Zn1 O1 C9 -84.8(4) 5_666 .
O4 Zn1 O1 C9 -4.4(7) 3_466 .
Zn1 Zn1 O1 C9 -4.0(4) 5_666 .
O5 C3 C4 C5 175.4(4) . .
C8 C3 C4 C5 -0.6(7) . .
C6 C5 C4 C3 -0.5(7) . .
C9 C5 C4 C3 -174.5(4) . .
C3 O5 C2 C1 -172.1(3) . .
C2 C1 C2 O5 -172.2(3) 15_656 .
C2 C1 C2 O5 -52.26(18) 16_666 .
C2 C1 C2 O5 67.8(3) 2_655 .
C4 C5 C6 C7 1.7(7) . .
C9 C5 C6 C7 175.7(4) . .
O5 C3 C8 C7 -175.8(4) . .
C4 C3 C8 C7 0.5(8) . .
C3 C8 C7 C6 0.7(7) . .
C3 C8 C7 C10 174.4(4) . .
C5 C6 C7 C8 -1.8(7) . .
C5 C6 C7 C10 -175.4(5) . .
Zn1 O1 C9 O2 -3.5(7) . .
Zn1 O1 C9 C5 179.0(3) . .
C6 C5 C9 O1 -179.3(4) . .
C4 C5 C9 O1 -5.3(6) . .
C6 C5 C9 O2 2.8(6) . .
C4 C5 C9 O2 176.9(4) . .
O1 C9 O2 Zn1 13.4(7) . 5_666
C5 C9 O2 Zn1 -169.0(3) . 5_666
C8 C7 C10 O3 10.0(7) . .
C6 C7 C10 O3 -176.4(5) . .
C8 C7 C10 O4 -170.4(4) . .
C6 C7 C10 O4 3.2(7) . .
O4 C10 O3 Zn1 16.8(9) . 8_655
C7 C10 O3 Zn1 -163.7(3) . 8_655
O3 C10 O4 Zn1 -8.4(7) . 3_566
C7 C10 O4 Zn1 172.1(3) . 3_566
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.017 -0.005 -0.002 5217.0 95.8
