#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/15/2011555.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_2011555
loop_
_publ_author_name
'Kongshaug, Kjell Ove'
'Fjellvåg, Helmer'
'Lillerud, Karl Petter'
_publ_section_title
;
 A three-dimensional open-framework zinc arsenate,
 (C₄H₁₂N₂)₂[Zn₇(AsO₄)₆(H₂O)₂]
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              e503
_journal_page_last               e504
_journal_paper_doi               10.1107/S0108270100013548
_journal_volume                  56
_journal_year                    2000
_chemical_formula_iupac          '(C4 H12 N2)2 [Zn7 (As O4)6 (H2 O)2]'
_chemical_formula_moiety         '2C4 H12 N2 2+, H4 As6 O26 Zn7 4-'
_chemical_formula_sum            'C8 H28 As6 N4 O26 Zn7'
_chemical_formula_weight         1503.455
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.564(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.5880(14)
_cell_length_b                   8.3559(7)
_cell_length_c                   23.4129(18)
_cell_measurement_reflns_used    3669
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3
_cell_volume                     3140.9(4)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        SAINT
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1994)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full .999
_diffrn_measured_fraction_theta_max .999
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method
'sets of exposures each taken over 0.6° ω rotation'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0793
_diffrn_reflns_av_sigmaI/netI    .0585
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            17378
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.54
_exptl_absorpt_coefficient_mu    11.636
_exptl_absorpt_correction_T_max  .55
_exptl_absorpt_correction_T_min  .26
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.179
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          .4
_exptl_crystal_size_mid          .1
_exptl_crystal_size_min          .05
_refine_diff_density_max         .872
_refine_diff_density_min         -.921
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   .947
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         3602
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      .947
_refine_ls_R_factor_all          .056
_refine_ls_R_factor_gt           .032
_refine_ls_shift/su_max          .001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0275P)²] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .065
_reflns_number_gt                2639
_reflns_number_total             3602
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            qa0423.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2011555
_cod_database_fobs_code          2011555
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_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_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
As1 .26918(3) .50999(7) .54802(2) .00799(12) Uani d . 1 . . As
As2 .05209(3) .28361(7) .13313(2) .00828(12) Uani d . 1 . . As
As3 .17838(3) .50461(7) .30936(2) .00834(12) Uani d . 1 . . As
Zn1 .30098(4) .65114(8) .42636(3) .00896(13) Uani d . 1 . . Zn
Zn2 -.14715(4) .35305(8) .07431(3) .00908(14) Uani d . 1 . . Zn
Zn3 .24056(4) .38125(8) .19269(3) .00976(14) Uani d . 1 . . Zn
Zn4 .0000 .30442(11) .2500 .00970(19) Uani d S 1 . . Zn
O1 .3245(2) .3634(5) .58939(16) .0159(8) Uani d . 1 . . O
O2 .1798(2) .4451(5) .50431(16) .0161(9) Uani d . 1 . . O
O3 .2507(2) .6421(5) .59762(16) .0115(8) Uani d . 1 . . O
O4 .3292(2) .6040(5) .50954(15) .0123(8) Uani d . 1 . . O
O5 .0935(2) .1434(5) .09622(16) .0121(8) Uani d . 1 . . O
O6 .0216(2) .1793(4) .18557(16) .0119(8) Uani d . 1 . . O
O7 -.0273(2) .3795(5) .08565(16) .0116(8) Uani d . 1 . . O
O8 .1224(2) .4234(4) .16244(16) .0115(8) Uani d . 1 . . O
O9 .2159(2) .4929(5) .38491(15) .0107(7) Uani d . 1 . . O
O10 .1931(3) .6885(5) .28760(16) .0158(8) Uani d . 1 . . O
O11 .0786(2) .4587(5) .29750(17) .0182(9) Uani d . 1 . . O
O12 .2335(2) .3720(5) .28051(15) .0124(8) Uani d . 1 . . O
OW .3168(3) .5693(5) .20120(17) .0138(8) Uani d . 1 . . O
N1 .4585(3) .2146(6) .0799(2) .0162(10) Uani d . 1 . . N
N2 .6076(3) .3471(6) .1519(2) .0136(10) Uani d . 1 . . N
C1 .5411(4) .2887(8) .1785(3) .0139(12) Uani d . 1 . . C
C2 .4585(4) .3062(7) .1344(3) .0152(12) Uani d . 1 . . C
C3 .5262(4) .7284(8) .5522(3) .0170(12) Uani d . 1 . . C
C4 .6086(4) .2555(7) .0968(3) .0155(12) Uani d . 1 . . C
H1 .413(4) .224(8) .055(3) .020 Uiso d . 1 . . H
H2 .470(4) .110(9) .092(3) .020 Uiso d . 1 . . H
H3 .602(4) .438(9) .143(3) .020 Uiso d . 1 . . H
H4 .663(4) .355(8) .173(3) .020 Uiso d . 1 . . H
H5 .555(4) .186(9) .196(3) .020 Uiso d . 1 . . H
H6 .543(4) .345(9) .209(3) .020 Uiso d . 1 . . H
H7 .412(4) .267(8) .154(3) .020 Uiso d . 1 . . H
H8 .448(4) .417(9) .126(3) .020 Uiso d . 1 . . H
H9 .514(4) .624(9) .543(3) .020 Uiso d . 1 . . H
H10 .526(4) .787(8) .522(3) .020 Uiso d . 1 . . H
H11 .621(4) .158(9) .107(3) .020 Uiso d . 1 . . H
H12 .648(4) .295(8) .084(3) .020 Uiso d . 1 . . H
H13 .304(4) .659(9) .218(3) .020 Uiso d . 1 . . H
H14 .322(4) .589(9) .171(3) .020 Uiso d . 1 . . H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn .2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As .0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 '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
_geom_angle_publ_flag
O2 As1 O1 . . 112.9(2) no
O2 As1 O3 . . 110.37(18) no
O1 As1 O3 . . 104.32(18) no
O2 As1 O4 . . 112.07(18) no
O1 As1 O4 . . 109.60(19) no
O3 As1 O4 . . 107.21(19) no
O8 As2 O6 . . 111.64(18) no
O8 As2 O7 . . 106.60(19) no
O6 As2 O7 . . 113.34(18) no
O8 As2 O5 . . 111.18(18) no
O6 As2 O5 . . 104.36(18) no
O7 As2 O5 . . 109.79(18) no
O11 As3 O10 . . 112.5(2) no
O11 As3 O12 . . 113.7(2) no
O10 As3 O12 . . 110.5(2) no
O11 As3 O9 . . 104.30(18) no
O10 As3 O9 . . 108.97(18) no
O12 As3 O9 . . 106.39(18) no
O4 Zn1 O3 . 7_566 116.76(16) no
O4 Zn1 O5 . 4 105.09(15) no
O3 Zn1 O5 7_566 4 108.09(16) no
O4 Zn1 O9 . . 108.56(16) no
O3 Zn1 O9 7_566 . 103.96(16) no
O5 Zn1 O9 4 . 114.75(16) no
O1 Zn2 O2 8_455 2 121.56(17) no
O1 Zn2 O7 8_455 . 111.70(17) no
O2 Zn2 O7 2 . 96.64(15) no
O1 Zn2 O9 8_455 2 105.21(16) no
O2 Zn2 O9 2 2 99.33(15) no
O7 Zn2 O9 . 2 122.97(16) no
O10 Zn3 O8 4_545 . 134.22(17) yes
O10 Zn3 OW 4_545 . 108.83(17) yes
O8 Zn3 OW . . 116.77(17) yes
O10 Zn3 O12 4_545 . 84.50(15) yes
O8 Zn3 O12 . . 93.67(15) yes
OW Zn3 O12 . . 97.00(16) yes
O10 Zn3 O3 4_545 6_565 89.12(15) yes
O8 Zn3 O3 . 6_565 88.56(14) yes
OW Zn3 O3 . 6_565 87.97(15) yes
O12 Zn3 O3 . 6_565 172.91(15) yes
O6 Zn4 O6 . 2 114.8(2) no
O6 Zn4 O11 . . 124.52(16) no
O6 Zn4 O11 2 . 97.99(16) no
O6 Zn4 O11 . 2 97.99(16) no
O6 Zn4 O11 2 2 124.52(16) no
O11 Zn4 O11 . 2 98.1(3) no
As1 O1 Zn2 . 8_556 134.5(2) no
As1 O2 Zn2 . 2 134.7(2) no
As1 O3 Zn1 . 7_566 121.7(2) no
As1 O3 Zn3 . 6_566 133.4(2) no
Zn1 O3 Zn3 7_566 6_566 102.84(16) no
As1 O4 Zn1 . . 127.3(2) no
As2 O5 Zn1 . 4_545 128.3(2) no
As2 O6 Zn4 . . 115.9(2) no
As2 O7 Zn2 . . 129.2(2) no
As2 O8 Zn3 . . 124.0(2) no
As3 O9 Zn1 . . 119.3(2) no
As3 O9 Zn2 . 2 114.48(18) no
Zn1 O9 Zn2 . 2 124.33(17) no
As3 O10 Zn3 . 4 144.7(2) no
As3 O11 Zn4 . . 137.8(2) no
As3 O12 Zn3 . . 122.8(2) no
Zn3 OW H13 . . 119(4) no
Zn3 OW H14 . . 108(6) no
H13 OW H14 . . 108(7) no
C2 N1 C3 . 6_565 111.5(5) no
C2 N1 H1 . . 111(5) no
C3 N1 H1 6_565 . 107(5) no
C2 N1 H2 . . 106(4) no
C3 N1 H2 6_565 . 108(4) no
H1 N1 H2 . . 113(6) no
C1 N2 C4 . . 111.4(5) no
C1 N2 H3 . . 112(5) no
C4 N2 H3 . . 107(5) no
C1 N2 H4 . . 123(4) no
C4 N2 H4 . . 105(4) no
H3 N2 H4 . . 96(6) no
N2 C1 C2 . . 108.9(5) no
N2 C1 H5 . . 111(4) no
C2 C1 H5 . . 118(4) no
N2 C1 H6 . . 107(5) no
C2 C1 H6 . . 111(4) no
H5 C1 H6 . . 100(6) no
N1 C2 C1 . . 110.1(5) no
N1 C2 H7 . . 112(4) no
C1 C2 H7 . . 108(3) no
N1 C2 H8 . . 111(4) no
C1 C2 H8 . . 109(4) no
H7 C2 H8 . . 106(5) no
C4 C3 N1 6_566 6_566 108.6(5) no
C4 C3 H9 6_566 . 111(4) no
N1 C3 H9 6_566 . 105(4) no
C4 C3 H10 6_566 . 109(4) no
N1 C3 H10 6_566 . 109(4) no
H9 C3 H10 . . 114(6) no
N2 C4 C3 . 6_565 110.2(5) no
N2 C4 H11 . . 107(4) no
C3 C4 H11 6_565 . 113(4) no
N2 C4 H12 . . 106(4) no
C3 C4 H12 6_565 . 112(4) no
H11 C4 H12 . . 109(6) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
As1 O2 . 1.667(4) no
As1 O1 . 1.683(4) no
As1 O3 . 1.686(4) no
As1 O4 . 1.695(4) no
As2 O8 . 1.671(4) no
As2 O6 . 1.684(4) no
As2 O7 . 1.696(4) no
As2 O5 . 1.699(4) no
As3 O11 . 1.653(4) no
As3 O10 . 1.656(4) no
As3 O12 . 1.682(4) no
As3 O9 . 1.724(3) no
Zn1 O4 . 1.926(4) no
Zn1 O3 7_566 1.947(4) no
Zn1 O5 4_555 1.953(4) no
Zn1 O9 . 1.998(4) no
Zn2 O1 8_455 1.924(4) no
Zn2 O2 2 1.942(4) no
Zn2 O7 . 1.951(4) no
Zn2 O9 2 2.031(4) no
Zn3 O10 4_545 1.940(4) yes
Zn3 O8 . 1.942(4) yes
Zn3 OW . 1.995(4) yes
Zn3 O12 . 2.090(4) yes
Zn3 O3 6_565 2.282(4) yes
Zn4 O6 . 1.941(4) no
Zn4 O6 2 1.941(4) no
Zn4 O11 . 1.967(4) no
Zn4 O11 2 1.967(4) no
O1 Zn2 8_556 1.924(4) no
O2 Zn2 2 1.942(4) no
O3 Zn1 7_566 1.947(4) no
O3 Zn3 6_566 2.282(4) no
O5 Zn1 4_545 1.953(4) no
O9 Zn2 2 2.031(4) no
O10 Zn3 4 1.940(4) no
OW H13 . .89(7) no
OW H14 . .74(7) no
N1 C2 . 1.488(8) no
N1 C3 6_565 1.507(8) no
N1 H1 . .83(7) no
N1 H2 . .93(7) no
N2 C1 . 1.480(7) no
N2 C4 . 1.503(8) no
N2 H3 . .79(7) no
N2 H4 . .93(7) no
C1 C2 . 1.502(8) no
C1 H5 . .95(7) no
C1 H6 . .85(7) no
C2 H7 . 1.04(6) no
C2 H8 . .96(7) no
C3 C4 6_566 1.504(8) no
C3 N1 6_566 1.507(8) no
C3 H9 . .91(7) no
C3 H10 . .85(7) no
C4 C3 6_565 1.504(8) no
C4 H11 . .86(7) no
C4 H12 . .85(7) no
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_1
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O2 As1 O1 Zn2 . 8_556 44.3(4) no
O3 As1 O1 Zn2 . 8_556 164.1(3) no
O4 As1 O1 Zn2 . 8_556 -81.4(3) no
O1 As1 O2 Zn2 . 2 -87.0(4) no
O3 As1 O2 Zn2 . 2 156.7(3) no
O4 As1 O2 Zn2 . 2 37.3(4) no
O2 As1 O3 Zn1 . 7_566 -65.5(3) no
O1 As1 O3 Zn1 . 7_566 173.0(2) no
O4 As1 O3 Zn1 . 7_566 56.8(3) no
O2 As1 O3 Zn3 . 6_566 95.0(3) no
O1 As1 O3 Zn3 . 6_566 -26.5(3) no
O4 As1 O3 Zn3 . 6_566 -142.7(3) no
O2 As1 O4 Zn1 . . 4.4(3) no
O1 As1 O4 Zn1 . . 130.5(3) no
O3 As1 O4 Zn1 . . -116.9(3) no
O3 Zn1 O4 As1 7_566 . 91.4(3) no
O5 Zn1 O4 As1 4 . -148.9(3) no
O9 Zn1 O4 As1 . . -25.7(3) no
O8 As2 O5 Zn1 . 4_545 -12.1(3) no
O6 As2 O5 Zn1 . 4_545 -132.6(3) no
O7 As2 O5 Zn1 . 4_545 105.6(3) no
O8 As2 O6 Zn4 . . 43.1(3) no
O7 As2 O6 Zn4 . . -77.2(2) no
O5 As2 O6 Zn4 . . 163.3(2) no
O6 Zn4 O6 As2 2 . -172.7(3) no
O11 Zn4 O6 As2 . . -52.4(3) no
O11 Zn4 O6 As2 2 . 53.2(2) no
O8 As2 O7 Zn2 . . -136.3(3) no
O6 As2 O7 Zn2 . . -13.0(3) no
O5 As2 O7 Zn2 . . 103.2(3) no
O1 Zn2 O7 As2 8_455 . -31.6(3) no
O2 Zn2 O7 As2 2 . -159.5(3) no
O9 Zn2 O7 As2 2 . 94.8(3) no
O6 As2 O8 Zn3 . . 82.2(3) no
O7 As2 O8 Zn3 . . -153.6(2) no
O5 As2 O8 Zn3 . . -33.9(3) no
O10 Zn3 O8 As2 4_545 . -13.6(4) no
OW Zn3 O8 As2 . . 160.8(2) no
O12 Zn3 O8 As2 . . -99.5(3) no
O3 Zn3 O8 As2 6_565 . 73.8(2) no
O11 As3 O9 Zn1 . . -142.4(2) no
O10 As3 O9 Zn1 . . -22.0(3) no
O12 As3 O9 Zn1 . . 97.1(2) no
O11 As3 O9 Zn2 . 2 22.7(3) no
O10 As3 O9 Zn2 . 2 143.0(2) no
O12 As3 O9 Zn2 . 2 -97.8(2) no
O4 Zn1 O9 As3 . . -179.9(2) no
O3 Zn1 O9 As3 7_566 . 55.2(2) no
O5 Zn1 O9 As3 4 . -62.7(3) no
O4 Zn1 O9 Zn2 . 2 16.7(3) no
O3 Zn1 O9 Zn2 7_566 2 -108.3(2) no
O5 Zn1 O9 Zn2 4 2 133.9(2) no
O11 As3 O10 Zn3 . 4 139.2(4) no
O12 As3 O10 Zn3 . 4 -92.5(4) no
O9 As3 O10 Zn3 . 4 24.0(5) no
O10 As3 O11 Zn4 . . 116.7(4) no
O12 As3 O11 Zn4 . . -9.9(4) no
O9 As3 O11 Zn4 . . -125.4(4) no
O6 Zn4 O11 As3 . . -14.3(5) no
O6 Zn4 O11 As3 2 . 113.4(4) no
O11 Zn4 O11 As3 2 . -119.9(4) no
O11 As3 O12 Zn3 . . 84.6(3) no
O10 As3 O12 Zn3 . . -43.0(3) no
O9 As3 O12 Zn3 . . -161.2(2) no
O10 Zn3 O12 As3 4_545 . -177.6(3) no
O8 Zn3 O12 As3 . . -43.5(3) no
OW Zn3 O12 As3 . . 74.0(3) no
O3 Zn3 O12 As3 6_565 . -151.7(10) no
C4 N2 C1 C2 . . -59.0(6) no
C3 N1 C2 C1 6_565 . -59.2(6) no
N2 C1 C2 N1 . . 58.5(6) no
C1 N2 C4 C3 . 6_565 59.2(6) no
