#------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/08/2240884.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2240884
loop_
_publ_author_name
'Ni, Min'
'Li, Quanle'
'Chen, Hao'
'Li, Shengqing'
_publ_section_title
;
 Crystal structure of [NaZn(BTC)(H₂O)₄]·1.5H₂O (BTC =
 benzene-1,3,5-tricarboxylate): a heterometallic coordination compound
;
_journal_coeditor_code           ZP2017
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m143
_journal_page_last               m144
_journal_paper_doi               10.1107/S2056989015012001
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Na Zn (C9 H3 O6) (H2 O)4], 1.5H2 O'
_chemical_formula_moiety         'C9 H11 Na O10 Zn, 1.5(H2 O)'
_chemical_formula_sum            'C9 H14 Na O11.5 Zn'
_chemical_formula_weight         394.56
_chemical_name_systematic
;
Poly[[μ-aqua-triaqua(μ₃-benzene-1,3,5-tricarboxylato)sodiumzinc]
sesquihydrate]
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
Olex2 1.2
(compiled 2014.12.26 svn.r3119 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                66.923(2)
_cell_angle_beta                 73.598(2)
_cell_angle_gamma                84.720(3)
_cell_formula_units_Z            2
_cell_length_a                   7.0980(11)
_cell_length_b                   9.8000(16)
_cell_length_c                   11.2043(17)
_cell_measurement_reflns_used    1047
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.53
_cell_measurement_theta_min      2.40
_cell_volume                     687.68(19)
_computing_cell_refinement
;
SAINT-Plus (Bruker, 2009)
;
_computing_data_collection
;
APEX2 (Bruker, 2009)
;
_computing_data_reduction
;
SAINT-Plus (Bruker, 2009)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al.,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al.,  2009)
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS7 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7585
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.044
_diffrn_reflns_theta_min         2.259
_exptl_absorpt_coefficient_mu    1.879
_exptl_absorpt_correction_T_max  0.9633
_exptl_absorpt_correction_T_min  0.9117
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2009)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.906
_exptl_crystal_density_method    ' not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             402
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.791
_refine_diff_density_min         -0.690
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         4331
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.1089
_refine_ls_R_factor_gt           0.0512
_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)+(0.0356P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0923
_refine_ls_wR_factor_ref         0.1130
_reflns_number_gt                2567
_reflns_number_total             4331
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            zp2017sup1.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C9 H14 Na O11.50 Zn'
_cod_database_code               2240884
_cod_database_fobs_code          2240884
#BEGIN Tags that were not found in dictionaries:
_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.
;
_shelx_estimated_absorpt_t_min   0.912
_shelx_estimated_absorpt_t_max   0.963
_shelxl_version_number           20.13
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn Zn1 0.69252(6) 1.17043(4) 0.17723(4) 0.02302(13) Uani d 1 . .
Na Na1 0.5000 1.0000 0.0000 0.0322(5) Uani d 1 . .
Na Na2 0.5000 0.0000 0.5000 0.0319(5) Uani d 1 . .
C C1 0.7424(5) 0.7068(3) 0.3327(3) 0.0184(7) Uani d 1 . .
C C2 0.7376(5) 0.5950(3) 0.2865(3) 0.0186(7) Uani d 1 . .
H H2 0.7312 0.6192 0.1988 0.022 Uiso calc 1 . .
C C3 0.7423(5) 0.4476(3) 0.3710(3) 0.0188(7) Uani d 1 . .
C C4 0.7512(5) 0.4130(4) 0.5013(3) 0.0207(7) Uani d 1 . .
H H4 0.7529 0.3140 0.5581 0.025 Uiso calc 1 . .
C C5 0.7576(5) 0.5231(4) 0.5492(3) 0.0211(7) Uani d 1 . .
C C6 0.7566(5) 0.6703(4) 0.4623(3) 0.0204(7) Uani d 1 . .
H H6 0.7657 0.7455 0.4917 0.024 Uiso calc 1 . .
C C7 0.7273(5) 0.8667(4) 0.2423(3) 0.0204(7) Uani d 1 . .
C C8 0.7345(5) 0.3229(4) 0.3272(3) 0.0206(7) Uani d 1 . .
C C9 0.7632(5) 0.4837(5) 0.6923(4) 0.0291(8) Uani d 1 . .
O O1 0.7044(4) 0.9607(3) 0.2967(3) 0.0371(7) Uani d 1 . .
O O2 0.7376(4) 0.8999(3) 0.1217(3) 0.0341(6) Uani d 1 . .
O O3 0.7335(4) 0.1931(3) 0.4071(3) 0.0325(6) Uani d 1 . .
O O4 0.7242(4) 0.3558(3) 0.2063(2) 0.0268(6) Uani d 1 . .
O O5 0.7596(4) 0.3477(4) 0.7661(3) 0.0467(8) Uani d 1 . .
O O6 0.7682(4) 0.5863(4) 0.7316(3) 0.0479(8) Uani d 1 . .
O O7 0.5762(4) 1.2363(3) 0.0195(2) 0.0292(6) Uani d 1 . .
H H7A 0.6483 1.2811 -0.0557 0.044 Uiso d 1 . .
H H7B 0.4703 1.2778 0.0249 0.044 Uiso d 1 . .
O O8 0.3875(4) 1.1497(3) 0.3061(3) 0.0396(7) Uani d 1 . .
H H8A 0.3040 1.0995 0.3031 0.059 Uiso d 1 . .
H H8B 0.3305 1.2022 0.3464 0.059 Uiso d 1 . .
O O9 0.9800(4) 1.1943(3) 0.0630(3) 0.0382(7) Uani d 1 . .
H H9A 1.0364 1.2580 0.0713 0.057 Uiso d 1 . .
H H9B 1.0536 1.1721 0.0026 0.057 Uiso d 1 . .
O O10 0.2322(5) 0.9423(4) 0.2021(4) 0.0790(13) Uani d 1 . .
H H10A 0.1808 0.8593 0.2402 0.119 Uiso d 1 . .
H H10B 0.1445 1.0027 0.1899 0.119 Uiso d 1 . .
O O11 0.0497(9) 0.9938(8) 0.4107(6) 0.0482(16) Uani d 0.5 A -1
H H11A -0.0558 1.0390 0.3993 0.072 Uiso d 0.5 A -1
H H11B 0.0429 0.9553 0.4942 0.072 Uiso d 0.5 A -1
O O12 0.7580(4) 0.6003(3) 0.9650(2) 0.0294(6) Uani d 1 . .
H H12A 0.7717 0.5773 0.9002 0.044 Uiso d 1 . .
H H12B 0.7499 0.5234 1.0318 0.044 Uiso d 1 . .
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'
Na Na 0.0362 0.0249 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
Na2 Zn1 Na1 1_565 . 108.751(15)
O1 Zn1 Na1 . . 81.47(8)
O1 Zn1 Na2 . 1_565 49.45(7)
O1 Zn1 O4 . 1_565 129.50(11)
O1 Zn1 O7 . . 123.49(11)
O1 Zn1 O8 . . 83.14(11)
O1 Zn1 O9 . . 97.22(11)
O4 Zn1 Na1 1_565 . 147.26(7)
O4 Zn1 Na2 1_565 1_565 89.66(7)
O4 Zn1 O7 1_565 . 105.44(10)
O4 Zn1 O8 1_565 . 88.15(11)
O4 Zn1 O9 1_565 . 89.49(10)
O7 Zn1 Na1 . . 42.24(7)
O7 Zn1 Na2 . 1_565 131.91(7)
O7 Zn1 O8 . . 86.91(10)
O7 Zn1 O9 . . 95.17(11)
O8 Zn1 Na1 . . 85.30(7)
O8 Zn1 Na2 . 1_565 47.48(7)
O9 Zn1 Na1 . . 97.50(8)
O9 Zn1 Na2 . 1_565 131.02(8)
O9 Zn1 O8 . . 177.20(11)
Zn1 Na1 Zn1 . 2_675 180.0
O2 Na1 Zn1 . . 53.49(6)
O2 Na1 Zn1 2_675 2_675 53.49(6)
O2 Na1 Zn1 2_675 . 126.51(6)
O2 Na1 Zn1 . 2_675 126.51(6)
O2 Na1 O2 2_675 . 180.0
O2 Na1 O7 2_675 2_675 83.14(8)
O2 Na1 O7 . . 83.14(8)
O2 Na1 O7 2_675 . 96.86(8)
O2 Na1 O7 . 2_675 96.86(8)
O2 Na1 O10 . 2_675 86.91(11)
O2 Na1 O10 2_675 2_675 93.09(11)
O2 Na1 O10 2_675 . 86.91(11)
O2 Na1 O10 . . 93.09(11)
O7 Na1 Zn1 2_675 . 147.65(5)
O7 Na1 Zn1 . . 32.36(5)
O7 Na1 Zn1 2_675 2_675 32.35(5)
O7 Na1 Zn1 . 2_675 147.64(5)
O7 Na1 O7 2_675 . 180.0
O10 Na1 Zn1 2_675 . 99.48(11)
O10 Na1 Zn1 . 2_675 99.48(11)
O10 Na1 Zn1 . . 80.52(11)
O10 Na1 Zn1 2_675 2_675 80.52(11)
O10 Na1 O7 . 2_675 89.62(12)
O10 Na1 O7 . . 90.38(12)
O10 Na1 O7 2_675 2_675 90.38(12)
O10 Na1 O7 2_675 . 89.62(12)
O10 Na1 O10 2_675 . 180.0
Zn1 Na2 Zn1 2_666 1_545 180.0
O1 Na2 Zn1 2_666 1_545 142.80(5)
O1 Na2 Zn1 1_545 1_545 37.20(5)
O1 Na2 Zn1 1_545 2_666 142.80(5)
O1 Na2 Zn1 2_666 2_666 37.20(5)
O1 Na2 O1 1_545 2_666 180.0
O3 Na2 Zn1 2_656 1_545 123.65(7)
O3 Na2 Zn1 . 1_545 56.35(7)
O3 Na2 Zn1 2_656 2_666 56.35(7)
O3 Na2 Zn1 . 2_666 123.65(7)
O3 Na2 O1 . 2_666 102.11(9)
O3 Na2 O1 . 1_545 77.89(9)
O3 Na2 O1 2_656 2_666 77.89(9)
O3 Na2 O1 2_656 1_545 102.11(9)
O3 Na2 O3 . 2_656 180.0
O3 Na2 O8 2_656 1_545 98.25(9)
O3 Na2 O8 2_656 2_666 81.75(9)
O3 Na2 O8 . 2_666 98.25(9)
O3 Na2 O8 . 1_545 81.75(9)
O8 Na2 Zn1 2_666 1_545 137.24(6)
O8 Na2 Zn1 1_545 2_666 137.24(6)
O8 Na2 Zn1 2_666 2_666 42.76(6)
O8 Na2 Zn1 1_545 1_545 42.76(6)
O8 Na2 O1 2_666 2_666 69.50(9)
O8 Na2 O1 2_666 1_545 110.50(9)
O8 Na2 O1 1_545 1_545 69.50(9)
O8 Na2 O1 1_545 2_666 110.50(9)
O8 Na2 O8 2_666 1_545 180.0
C2 C1 C7 . . 119.8(3)
C6 C1 C2 . . 119.7(3)
C6 C1 C7 . . 120.6(3)
C1 C2 H2 . . 119.9
C3 C2 C1 . . 120.1(3)
C3 C2 H2 . . 119.9
C2 C3 C8 . . 122.3(3)
C4 C3 C2 . . 119.4(3)
C4 C3 C8 . . 118.2(3)
C3 C4 H4 . . 119.3
C3 C4 C5 . . 121.4(3)
C5 C4 H4 . . 119.3
C4 C5 C9 . . 120.8(3)
C6 C5 C4 . . 118.3(3)
C6 C5 C9 . . 120.8(3)
C1 C6 C5 . . 121.0(3)
C1 C6 H6 . . 119.5
C5 C6 H6 . . 119.5
O1 C7 C1 . . 116.3(3)
O2 C7 C1 . . 120.1(3)
O2 C7 O1 . . 123.6(3)
O3 C8 C3 . . 120.1(3)
O3 C8 O4 . . 122.0(3)
O4 C8 C3 . . 117.9(3)
O5 C9 C5 . . 117.2(4)
O6 C9 C5 . . 118.8(4)
O6 C9 O5 . . 124.0(4)
Zn1 O1 Na2 . 1_565 93.35(9)
C7 O1 Zn1 . . 116.3(2)
C7 O1 Na2 . 1_565 140.1(2)
C7 O2 Na1 . . 130.6(2)
C8 O3 Na2 . . 132.2(2)
C8 O4 Zn1 . 1_545 110.2(2)
Zn1 O7 Na1 . . 105.40(10)
Zn1 O7 H7A . . 117.9
Zn1 O7 H7B . . 118.8
Na1 O7 H7A . . 101.6
Na1 O7 H7B . . 102.9
H7A O7 H7B . . 107.7
Zn1 O8 Na2 . 1_565 89.76(9)
Zn1 O8 H8A . . 121.4
Zn1 O8 H8B . . 129.0
Na2 O8 H8A 1_565 . 106.3
Na2 O8 H8B 1_565 . 89.2
H8A O8 H8B . . 107.7
Zn1 O9 H9A . . 109.9
Zn1 O9 H9B . . 141.4
H9A O9 H9B . . 107.7
Na1 O10 H10A . . 120.4
Na1 O10 H10B . . 110.7
H10A O10 H10B . . 107.7
H11A O11 H11B . . 109.5
H12A O12 H12B . . 107.7
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Zn1 Na1 . 3.6267(5)
Zn1 Na2 1_565 3.2603(6)
Zn1 O1 . 1.975(2)
Zn1 O4 1_565 2.009(2)
Zn1 O7 . 2.013(2)
Zn1 O8 . 2.214(3)
Zn1 O9 . 2.058(3)
Na1 Zn1 2_675 3.6267(5)
Na1 O2 . 2.369(3)
Na1 O2 2_675 2.369(3)
Na1 O7 . 2.529(3)
Na1 O7 2_675 2.529(3)
Na1 O10 . 2.413(3)
Na1 O10 2_675 2.413(3)
Na2 Zn1 2_666 3.2603(6)
Na2 Zn1 1_545 3.2603(6)
Na2 O1 1_545 2.482(2)
Na2 O1 2_666 2.482(2)
Na2 O3 . 2.339(3)
Na2 O3 2_656 2.339(3)
Na2 O8 2_666 2.403(3)
Na2 O8 1_545 2.403(3)
C1 C2 . 1.389(4)
C1 C6 . 1.384(4)
C1 C7 . 1.509(4)
C2 H2 . 0.9300
C2 C3 . 1.386(4)
C3 C4 . 1.382(4)
C3 C8 . 1.495(4)
C4 H4 . 0.9300
C4 C5 . 1.390(5)
C5 C6 . 1.390(4)
C5 C9 . 1.506(5)
C6 H6 . 0.9300
C7 O1 . 1.267(4)
C7 O2 . 1.242(4)
C8 O3 . 1.235(4)
C8 O4 . 1.286(4)
C9 O5 . 1.262(5)
C9 O6 . 1.252(5)
O1 Na2 1_565 2.482(2)
O4 Zn1 1_545 2.009(2)
O7 H7A . 0.8201
O7 H7B . 0.8201
O8 Na2 1_565 2.403(3)
O8 H8A . 0.8200
O8 H8B . 0.8201
O9 H9A . 0.8199
O9 H9B . 0.8200
O10 H10A . 0.8200
O10 H10B . 0.8200
O11 H11A . 0.8500
O11 H11B . 0.8500
O12 H12A . 0.8203
O12 H12B . 0.8200
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O7 H7A O5 1_564 0.82 1.79 2.587(4) 162
O7 H7B O12 2_676 0.82 1.93 2.740(4) 172
O8 H8A O10 . 0.82 2.40 3.114(5) 146
O8 H8A O11 . 0.82 1.98 2.672(8) 142
O8 H8B O6 2_676 0.82 2.05 2.641(5) 128
O9 H9A O12 2_776 0.82 1.95 2.734(4) 159
O9 H9B O2 2_775 0.82 2.01 2.823(4) 170
O10 H10A O5 2_666 0.82 2.06 2.719(6) 137
O10 H10B O9 1_455 0.82 2.31 3.079(5) 155
O11 H11A O3 1_465 0.85 2.03 2.835(8) 157
O11 H11B O3 2_666 0.85 2.27 2.866(7) 127
O11 H11B O11 2_576 0.85 1.33 1.973(9) 128
O12 H12A O6 1_555 0.82 1.86 2.652(4) 161
O12 H12B O4 1_556 0.82 1.97 2.787(3) 172
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_site_symmetry_4
_geom_torsion
C1 C2 C3 C4 . 0.2(5)
C1 C2 C3 C8 . 179.1(3)
C1 C7 O1 Zn1 . 178.2(2)
C1 C7 O1 Na2 1_565 -48.0(5)
C1 C7 O2 Na1 . 114.6(3)
C2 C1 C6 C5 . -2.8(5)
C2 C1 C7 O1 . 170.3(3)
C2 C1 C7 O2 . -9.9(5)
C2 C3 C4 C5 . -0.7(5)
C2 C3 C8 O3 . -178.0(3)
C2 C3 C8 O4 . 0.4(5)
C3 C4 C5 C6 . -0.6(5)
C3 C4 C5 C9 . 178.8(3)
C3 C8 O3 Na2 . 116.2(3)
C3 C8 O4 Zn1 1_545 -175.2(2)
C4 C3 C8 O3 . 0.9(5)
C4 C3 C8 O4 . 179.3(3)
C4 C5 C6 C1 . 2.3(5)
C4 C5 C9 O5 . -0.8(5)
C4 C5 C9 O6 . -179.8(3)
C6 C1 C2 C3 . 1.5(5)
C6 C1 C7 O1 . -8.3(5)
C6 C1 C7 O2 . 171.6(3)
C6 C5 C9 O5 . 178.5(3)
C6 C5 C9 O6 . -0.4(5)
C7 C1 C2 C3 . -177.0(3)
C7 C1 C6 C5 . 175.7(3)
C8 C3 C4 C5 . -179.6(3)
C9 C5 C6 C1 . -177.1(3)
O1 C7 O2 Na1 . -65.6(4)
O2 C7 O1 Zn1 . -1.6(5)
O2 C7 O1 Na2 1_565 132.1(3)
O3 C8 O4 Zn1 1_545 3.1(4)
O4 C8 O3 Na2 . -62.1(5)
