The salt of the di-μ-chloro-bis[tetrachlorozirconium(IV)] anion with protonated 1,3,5-trimethoxybenzene as cation
Coles, Simon J.; Hursthouse, Michael B.; Kelly, David G.; Walker, Neil M.; Acta Crystallographica Section C 55 (1999) 1789–1791; doi:10.1107/S0108270199010355

data_2009106
_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_paper_doi               10.1107/S0108270199010355
_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_details
'w = 1/[\s^2^(Fo^2^)+(0.0282P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.147
_reflns_number_gt                1529
_reflns_number_total             2334
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cf1324.cif
_cod_data_source_block           s92
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0282P)^2^] where P = (Fo^2^+2Fc^2^)/3' was changed
to 'calc'. New tag '_refine_ls_weighting_details' was created. The
value of the new tag was set to 'w = 1/[\s^2^(Fo^2^)+(0.0282P)^2^]
where P = (Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2009106
_cod_database_fobs_code          2009106