#------------------------------------------------------------------------------
#$Date: 2019-11-24 12:54:08 +0200 (Sun, 24 Nov 2019) $
#$Revision: 237950 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/35/00/4350027.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_4350027
loop_
_publ_author_name
'Liu, Zhanning'
'Jiang, Xingxing'
'Wang, Chiming'
'Liu, Chenxi'
'Lin, Zheshuai'
'Deng, Jinxia'
'Chen, Jun'
'Xing, Xianran'
_publ_section_title
;
 Near-zero thermal expansion coordinated with geometric flexibility and
 π⋯π interaction in anisotropic [Zn8(SiO4)(m-BDC)6]n
;
_journal_issue                   7
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              1675
_journal_paper_doi               10.1039/C9QI00354A
_journal_volume                  6
_journal_year                    2019
_chemical_formula_moiety         '0.5(C96 H48 O56 Si2 Zn16)'
_chemical_formula_sum            'C48 H24 O28 Si Zn8'
_chemical_formula_weight         1599.72
_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-03-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2018-03-06 deposited with the CCDC.	2019-05-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.69968(18)
_cell_length_b                   13.69968(18)
_cell_length_c                   15.0187(3)
_cell_measurement_reflns_used    2805
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      67.2730
_cell_measurement_theta_min      3.2050
_cell_volume                     2818.73(8)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      299(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0166
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4698
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.189
_diffrn_reflns_theta_max         67.189
_diffrn_reflns_theta_min         4.368
_exptl_absorpt_coefficient_mu    4.692
_exptl_absorpt_correction_T_max  0.45
_exptl_absorpt_correction_T_min  0.391
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.885
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bulk
_exptl_crystal_F_000             1580
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         2491
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.172
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0322
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0374P)²+3.9070P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0840
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2378
_reflns_number_total             2491
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9qi00354a2.cif
_cod_data_source_block           300k_sq_sq
_cod_original_cell_volume        2818.73(9)
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               4350027
_shelx_shelxl_version_number     2016/6
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C4(H4), C1AA(H1AA), C0AA(H0AA), C3AA(H3AA), C4AA(H4AA), C5AA(H5AA)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z'
'y+1/2, -x, z+1/2'
'-x, -y, -z'
'y, -x-1/2, -z-1/2'
'x-1/2, y-1/2, -z'
'-y-1/2, x, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Zn1 Zn 0.61768(3) 0.61518(3) 0.12347(3) 0.01911(13) Uani 1 1 d . . .
Zn2 Zn 0.54110(3) 0.81706(3) 0.17512(3) 0.01796(13) Uani 1 1 d . . .
Si3 Si 0.750000 0.750000 0.250000 0.0141(3) Uani 1 4 d S T P
O3 O 0.65307(15) 0.73175(15) 0.19012(14) 0.0189(4) Uani 1 1 d . . .
O1 O 0.49744(18) 0.56722(19) 0.17785(15) 0.0316(6) Uani 1 1 d . . .
O2 O 0.5590(2) 0.95740(16) 0.17917(16) 0.0310(6) Uani 1 1 d . . .
O0AA O 0.5764(2) 0.65763(18) 0.00722(16) 0.0358(6) Uani 1 1 d . . .
O4 O 0.42902(17) 0.78738(19) 0.25167(16) 0.0321(6) Uani 1 1 d . . .
O5 O 0.50790(19) 0.79770(18) 0.04985(15) 0.0327(6) Uani 1 1 d . . .
O6 O 0.7024(2) 0.50462(18) 0.11695(18) 0.0359(6) Uani 1 1 d . . .
C5 C 0.5334(2) 0.7372(2) -0.0079(2) 0.0246(7) Uani 1 1 d . . .
C7 C 0.5130(2) 0.7614(2) -0.1029(2) 0.0240(7) Uani 1 1 d . . .
C11 C 0.5230(3) 0.6902(3) -0.1683(2) 0.0369(9) Uani 1 1 d . . .
H11 H 0.542144 0.627302 -0.152790 0.044 Uiso 1 1 calc R . .
C4 C 0.4860(2) 0.8554(2) -0.1261(2) 0.0226(6) Uani 1 1 d . . .
H4 H 0.478339 0.902943 -0.082438 0.027 Uiso 1 1 calc R . .
C1AA C 0.4792(3) 0.8070(3) -0.2795(2) 0.0330(8) Uani 1 1 d . . .
H1AA H 0.468023 0.822650 -0.338927 0.040 Uiso 1 1 calc R . .
C0AA C 0.5045(4) 0.7130(3) -0.2564(2) 0.0433(10) Uani 1 1 d . . .
H0AA H 0.509129 0.664965 -0.299985 0.052 Uiso 1 1 calc R . .
C2 C 0.4704(2) 0.8781(2) -0.2148(2) 0.0213(6) Uani 1 1 d . . .
C1 C 0.5545(2) 1.0194(2) 0.2407(2) 0.0218(6) Uani 1 1 d . . .
C3 C 0.4300(2) 0.7853(2) 0.3351(2) 0.0262(7) Uani 1 1 d . . .
C2AA C 0.3364(2) 0.7657(3) 0.3830(2) 0.0258(7) Uani 1 1 d . . .
C3AA C 0.250000 0.750000 0.3365(3) 0.0226(9) Uani 1 2 d S T P
H3AA H 0.250001 0.749998 0.274579 0.027 Uiso 1 2 calc RS T P
C4AA C 0.3354(3) 0.7656(4) 0.4752(3) 0.0464(11) Uani 1 1 d . . .
H4AA H 0.393086 0.776225 0.506383 0.056 Uiso 1 1 calc R . .
C5AA C 0.250000 0.750000 0.5210(4) 0.063(2) Uani 1 2 d S T P
H5AA H 0.250001 0.749998 0.582877 0.075 Uiso 1 2 calc RS T P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 '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
O3 Zn1 Zn2 38.08(6) . .
O3 Zn1 O1 105.74(10) . .
O1 Zn1 Zn2 84.77(8) . .
O0AA Zn1 Zn2 81.72(7) . .
O0AA Zn1 O3 106.96(10) . .
O0AA Zn1 O1 103.48(12) . .
O6 Zn1 Zn2 159.79(9) . .
O6 Zn1 O3 121.72(11) . .
O6 Zn1 O1 105.49(11) . .
O6 Zn1 O0AA 111.80(11) . .
O3 Zn2 Zn1 38.19(6) . .
O3 Zn2 O4 115.20(10) . .
O3 Zn2 O5 102.35(9) . .
O2 Zn2 Zn1 149.45(8) . .
O2 Zn2 O3 119.55(10) . .
O2 Zn2 O4 106.64(11) . .
O2 Zn2 O5 101.20(10) . .
O4 Zn2 Zn1 103.29(8) . .
O5 Zn2 Zn1 73.31(7) . .
O5 Zn2 O4 110.74(11) . .
O3 Si3 O3 107.88(7) 3_665 8_756
O3 Si3 O3 107.88(7) . 8_756
O3 Si3 O3 112.71(15) . 3_665
O3 Si3 O3 112.71(15) 6_576 8_756
O3 Si3 O3 107.88(7) 6_576 3_665
O3 Si3 O3 107.88(7) . 6_576
Zn2 O3 Zn1 103.73(9) . .
Si3 O3 Zn1 127.97(12) . .
Si3 O3 Zn2 128.17(12) . .
C1 O1 Zn1 127.5(2) 8_756 .
C1 O2 Zn2 133.4(2) . .
C5 O0AA Zn1 124.2(2) . .
C3 O4 Zn2 125.6(2) . .
C5 O5 Zn2 133.9(2) . .
C3 O6 Zn1 134.0(2) 8_756 .
O0AA C5 C7 116.9(3) . .
O5 C5 O0AA 125.5(3) . .
O5 C5 C7 117.6(3) . .
C11 C7 C5 120.1(3) . .
C4 C7 C5 119.9(3) . .
C4 C7 C11 120.0(3) . .
C0AA C11 C7 120.0(3) . .
C7 C4 C2 119.5(3) . .
C0AA C1AA C2 120.3(3) . .
C1AA C0AA C11 119.9(3) . .
C4 C2 C1 119.7(3) . 5_675
C1AA C2 C4 120.3(3) . .
C1AA C2 C1 120.0(3) . 5_675
O1 C1 C2 117.1(3) 6_576 5_675
O2 C1 O1 125.8(3) . 6_576
O2 C1 C2 117.0(3) . 5_675
O4 C3 O6 125.2(3) . 6_576
O4 C3 C2AA 118.4(3) . .
O6 C3 C2AA 116.4(3) 6_576 .
C3AA C2AA C3 121.1(3) . .
C4AA C2AA C3 119.3(3) . .
C4AA C2AA C3AA 119.6(3) . .
C2AA C3AA C2AA 119.7(4) 3_565 .
C5AA C4AA C2AA 120.6(4) . .
C4AA C5AA C4AA 120.0(5) 3_565 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 Zn2 3.0580(5) .
Zn1 O3 1.946(2) .
Zn1 O1 1.952(2) .
Zn1 O0AA 1.925(2) .
Zn1 O6 1.910(2) .
Zn2 O3 1.942(2) .
Zn2 O2 1.939(2) .
Zn2 O4 1.961(2) .
Zn2 O5 1.954(2) .
Si3 O3 1.623(2) .
Si3 O3 1.623(2) 8_756
Si3 O3 1.623(2) 6_576
Si3 O3 1.623(2) 3_665
O1 C1 1.257(4) 8_756
O2 C1 1.256(4) .
O0AA C5 1.259(4) .
O4 C3 1.254(4) .
O5 C5 1.249(4) .
O6 C3 1.261(4) 8_756
C5 C7 1.491(4) .
C7 C11 1.391(5) .
C7 C4 1.385(5) .
C11 C0AA 1.383(5) .
C4 C2 1.385(4) .
C1AA C0AA 1.379(5) .
C1AA C2 1.381(5) .
C2 C1 1.496(4) 5_675
C3 C2AA 1.495(5) .
C2AA C3AA 1.391(4) .
C2AA C4AA 1.384(5) .
C4AA C5AA 1.374(5) .
