#------------------------------------------------------------------------------
#$Date: 2011-09-10 05:16:28 +0200 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2009106.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_2009106
loop_
_publ_author_name
'Coles, S. J.'
'Hursthouse, M. B.'
'Kelly, D. G.'
_publ_section_title
;
 The salt of the di-\m-chloro-bis[tetrachlorozirconium(IV)] anion with
 protonated 1,3,5-trimethoxybenzene as cation
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1789
_journal_page_last               1791
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac          '(C9 H13 O3)2 [Zr2 Cl10]'
_chemical_formula_moiety         '2C9 H13 O3 1+, Zr2 Cl10 2-'
_chemical_formula_sum            'C9 H13 Cl5 O3 Zr'
_chemical_formula_weight         875.34
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 110.079(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.905(2)
_cell_length_b                   9.9448(14)
_cell_length_c                   14.8508(15)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.14
_cell_measurement_theta_min      3.29
_cell_volume                     1651.4(4)
_computing_cell_refinement       MADNES
_computing_data_collection       'MADNES (Pflugrath & Messerschmidt, 1989)'
_computing_data_reduction        'ABSMAD (Karaulov, 1992)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1995)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997b)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_measurement_device
;
Nonius FAST TV area-detector diffractometer with an Oxford Cryosystems
Cryostream cooler (Cosier & Glazer, 1986)
;
_diffrn_measurement_method       \w
_diffrn_radiation_source         'Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0953
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5931
_diffrn_reflns_theta_full
;
The data set is no more than 91.9% complete for any theta(max) value.
This is due to a blind spot in the dataset, despite a data collection strategy
that involved two chi settings and was computed to cover a hemisphere of
reciprocal space. Zero and negative intensity reflections were included and
no weak high angle data were omitted.
;
_diffrn_reflns_theta_max         24.29
_diffrn_reflns_theta_min         1.9
_exptl_absorpt_coefficient_mu    1.47
_exptl_absorpt_correction_T_max  0.855
_exptl_absorpt_correction_T_min  0.684
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   '(DIFABS; Walker & Stuart, 1983)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.756
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.703
_refine_diff_density_min         -0.636
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         2324
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.557
_refine_ls_R_factor_gt           0.036
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w = 1/[\s^2^(Fo^2^)+(0.0282P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_ref         0.147
_reflns_number_gt                1529
_reflns_number_total             2334
_reflns_threshold_expression     I>2\s(I)
_[local]_cod_data_source_file    cf1324.cif
_[local]_cod_data_source_block   s92
_[local]_cod_cif_authors_sg_H-M  'P 21/n'
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2009106
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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_type_symbol
Zr1 0.87572(4) 0.07016(5) 0.05364(4) 0.0206(2) Uani d . 1 Zr
Cl2 0.82850(11) 0.24005(12) -0.07109(10) 0.0260(3) Uani d . 1 Cl
Cl3 0.94427(12) -0.09521(14) 0.18014(10) 0.0332(4) Uani d . 1 Cl
Cl4 1.09828(10) 0.10300(12) 0.07057(10) 0.0221(3) Uani d . 1 Cl
Cl5 0.67394(11) -0.00645(14) 0.00750(11) 0.0318(4) Uani d . 1 Cl
Cl6 0.87956(13) 0.24057(14) 0.16868(11) 0.0378(4) Uani d . 1 Cl
O1 0.8530(3) 0.5731(3) -0.1127(3) 0.0250(9) Uani d . 1 O
O2 0.5327(3) 0.6630(3) -0.0066(3) 0.0363(11) Uani d . 1 O
O3 0.9245(3) 0.5748(4) 0.2147(3) 0.0295(9) Uani d . 1 O
C1 0.8892(4) 0.5726(5) 0.0514(4) 0.0205(12) Uani d . 1 C
H1 0.9690(4) 0.5508(5) 0.0633(4) 0.025 Uiso calc R 1 H
C2 0.8029(4) 0.5901(5) -0.0473(4) 0.0226(13) Uani d . 1 C
C3 0.6851(5) 0.6193(5) -0.0635(4) 0.0253(13) Uani d . 1 C
H3 0.6312(5) 0.6291(5) -0.1256(4) 0.03 Uiso calc R 1 H
C4 0.6475(4) 0.6341(5) 0.0168(4) 0.0252(14) Uani d . 1 C
C5 0.7232(4) 0.6210(5) 0.1126(4) 0.0280(14) Uani d . 1 C
H5 0.6947(4) 0.6317(5) 0.1632(4) 0.034 Uiso calc R 1 H
C6 0.8412(5) 0.5916(5) 0.1283(4) 0.0235(13) Uani d . 1 C
C7 0.7806(5) 0.5856(6) -0.2100(4) 0.046(2) Uani d . 1 C
H7A 0.8292(8) 0.576(4) -0.2495(4) 0.069 Uiso calc R 1 H
H7B 0.743(3) 0.6722(16) -0.2205(7) 0.069 Uiso calc R 1 H
H7C 0.720(2) 0.517(2) -0.2261(8) 0.069 Uiso calc R 1 H
C8 0.4835(5) 0.6861(6) 0.0675(5) 0.039(2) Uani d . 1 C
H8A 0.3994(7) 0.704(3) 0.0392(5) 0.058 Uiso calc R 1 H
H8B 0.522(2) 0.762(2) 0.1053(16) 0.058 Uiso calc R 1 H
H8C 0.496(3) 0.6079(14) 0.1076(15) 0.058 Uiso calc R 1 H
C9 0.8894(5) 0.5841(6) 0.2971(4) 0.046(2) Uani d . 1 C
H9A 0.9566(9) 0.564(4) 0.3535(5) 0.068 Uiso calc R 1 H
H9B 0.826(2) 0.521(3) 0.2915(13) 0.068 Uiso calc R 1 H
H9C 0.862(3) 0.6735(11) 0.3019(15) 0.068 Uiso calc R 1 H
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Zr1 0.0182(3) 0.0209(3) 0.0217(3) -0.0014(2) 0.0056(2) -0.0007(2)
Cl2 0.0271(8) 0.0225(8) 0.0260(9) 0.0043(5) 0.0060(6) 0.0034(6)
Cl3 0.0349(9) 0.0323(9) 0.0273(9) -0.0046(6) 0.0043(6) 0.0083(6)
Cl4 0.0188(7) 0.0208(8) 0.0239(8) -0.0022(5) 0.0039(5) -0.0026(6)
Cl5 0.0199(8) 0.0385(9) 0.0360(10) -0.0050(6) 0.0084(6) -0.0042(7)
Cl6 0.0555(10) 0.0291(10) 0.0344(10) -0.0075(7) 0.0227(7) -0.0086(7)
O1 0.023(2) 0.031(2) 0.020(2) 0.003(2) 0.006(2) 0.002(2)
O2 0.019(2) 0.037(3) 0.051(3) 0.003(2) 0.010(2) 0.001(2)
O3 0.027(2) 0.041(2) 0.019(2) 0.005(2) 0.006(2) 0.003(2)
C1 0.013(3) 0.029(3) 0.017(3) 0.005(2) 0.002(2) 0.003(2)
C2 0.023(3) 0.015(3) 0.028(4) -0.003(2) 0.005(3) -0.003(2)
C3 0.025(3) 0.023(3) 0.024(4) 0.000(2) 0.003(3) 0.001(3)
C4 0.013(3) 0.017(3) 0.041(4) -0.002(2) 0.003(3) 0.001(3)
C5 0.023(3) 0.026(4) 0.034(4) -0.001(2) 0.009(3) 0.002(3)
C6 0.030(3) 0.013(3) 0.026(4) 0.001(2) 0.008(3) 0.005(2)
C7 0.049(4) 0.065(5) 0.022(4) 0.007(3) 0.009(3) 0.001(3)
C8 0.025(3) 0.041(4) 0.054(5) 0.006(3) 0.018(3) -0.001(3)
C9 0.034(4) 0.077(5) 0.024(4) 0.013(3) 0.006(3) 0.002(3)
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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 '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_3
_geom_angle
_geom_angle_publ_flag
Cl5 Zr1 Cl6 . 101.63(5) yes
Cl5 Zr1 Cl3 . 92.52(5) ?
Cl6 Zr1 Cl3 . 90.48(5) ?
Cl5 Zr1 Cl2 . 93.24(5) ?
Cl6 Zr1 Cl2 . 89.69(5) ?
Cl3 Zr1 Cl2 . 174.08(5) yes
Cl5 Zr1 Cl4 . 164.18(5) ?
Cl6 Zr1 Cl4 . 94.19(5) ?
Cl3 Zr1 Cl4 . 87.09(5) ?
Cl2 Zr1 Cl4 . 87.00(4) ?
Cl5 Zr1 Cl4 3_755 86.48(5) ?
Cl6 Zr1 Cl4 3_755 171.77(5) ?
Cl3 Zr1 Cl4 3_755 90.58(5) ?
Cl2 Zr1 Cl4 3_755 88.43(5) ?
Cl4 Zr1 Cl4 3_755 77.72(4) yes
Zr1 Cl4 Zr1 3_755 102.28(4) ?
C2 O1 C7 . 118.2(4) ?
C4 O2 C8 . 119.5(5) ?
C6 O3 C9 . 118.5(4) ?
C6 C1 C2 . 115.8(4) ?
O1 C2 C3 . 126.5(5) ?
O1 C2 C1 . 112.3(4) ?
C3 C2 C1 . 121.3(5) ?
C2 C3 C4 . 118.3(5) ?
O2 C4 C5 . 122.2(5) ?
O2 C4 C3 . 113.4(5) ?
C5 C4 C3 . 124.4(5) ?
C6 C5 C4 . 117.0(6) ?
O3 C6 C5 . 124.7(5) ?
O3 C6 C1 . 112.1(4) ?
C5 C6 C1 . 123.3(5) ?
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
Zr1 Cl5 . 2.3856(14) yes
Zr1 Cl6 . 2.396(2) yes
Zr1 Cl3 . 2.4181(15) yes
Zr1 Cl2 . 2.4263(14) yes
Zr1 Cl4 . 2.5949(13) yes
Zr1 Cl4 3_755 2.6184(14) yes
Cl4 Zr1 3_755 2.6184(14) ?
O1 C2 . 1.314(6) ?
O1 C7 . 1.411(6) ?
O2 C4 . 1.322(6) ?
O2 C8 . 1.431(7) ?
O3 C6 . 1.336(6) ?
O3 C9 . 1.425(7) ?
C1 C6 . 1.456(7) ?
C1 C2 . 1.483(7) ?
C2 C3 . 1.370(7) ?
C3 C4 . 1.418(8) ?
C4 C5 . 1.404(7) ?
C5 C6 . 1.374(7) ?