Preparation and X-ray Crystal Structure of the Polymeric Zirconium(IV) Oxalate Complex [K2{Zr(C2O4)3}.H2C2O4.H2O]n
Ricardo Baggio; Maria Teresa Garland; Mireille Perec; Inorganic Chemistry 36 (1997) 737–739; doi:10.1021/ic960987z

data_4323315
_publ_section_title
;
 Preparation and X-ray Crystal Structure of the Polymeric Zirconium(IV)
 Oxalate Complex [K2{Zr(C2O4)3}.H2C2O4.H2O]n
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              737
_journal_page_last               739
_journal_paper_doi               10.1021/ic960987z
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C8 H4 K2 O17 Zr'
_chemical_formula_weight         541.53
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 107.93(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.465(5)
_cell_length_b                   11.149(3)
_cell_length_c                   8.939(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      7.5
_cell_volume                     1561.2(8)
_computing_cell_refinement       'Siemens P3/P4-PC version V4.27 (1991)'
_computing_data_collection       'Siemens P3/P4-PC version V4.27 (1991)'
_computing_data_reduction        'XDISK in SHELXTL/PC(Sheldrick,1991)'
_computing_molecular_graphics    'XP in SHELXTL/PC(Sheldrick,1991)'
_computing_publication_material
;
CIFTAB (Sheldrick, 1993), PARST (Nardelli, 1983) and
CSD (Allen, Kennard & Taylor, 1983)
;
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens R3m'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2362
_diffrn_reflns_theta_max         28.49
_diffrn_reflns_theta_min         2.24
_diffrn_standards_decay_%        <2
_diffrn_standards_interval_count 98
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.337
_exptl_absorpt_correction_T_max  0.916
_exptl_absorpt_correction_T_min  0.724
_exptl_absorpt_correction_type   'Semiempirical ( Psi-scan)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.304
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Polyhedra
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.07(7)
_refine_ls_extinction_coef       0.0001(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.114
_refine_ls_goodness_of_fit_obs   1.121
_refine_ls_hydrogen_treatment    ' Riding on host atom'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         2154
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.152
_refine_ls_restrained_S_obs      1.162
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_obs          0.0291
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+2.4262P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0691
_refine_ls_wR_factor_obs         0.0667
_reflns_number_observed          1902
_reflns_number_total             2154
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960987z.cif
_cod_data_source_block           Zr_K_Oxal
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to the
built-in table from CIF Core dictionary named 'cif_core.dic' version
2.4.1 from 2010-06-29 (47 times).

'_geom_angle_publ_flag' value 'Y'
changed to 'y' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (142
times).

'_geom_torsion_publ_flag' value 'N' changed to 'n' according
to the built-in table from CIF Core dictionary named 'cif_core.dic'
version 2.4.1 from 2010-06-29 (16 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+2.4262P] 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^)+(0.0305P)^2^+2.4262P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4323315