#------------------------------------------------------------------------------
#$Date: 2025-08-21 03:34:05 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301843 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/79/4517900.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4517900
loop_
_publ_author_name
'Thomas, Rudy'
'Devaux, Philippe'
'Rivenet, Murielle'
'Henry, Natacha'
'Abraham, Francis'
_publ_section_title
;
 Zirconium Oxalates: Zr(OH)₂(C₂O₄),
 (H₁₁O₅)₂[Zr₂(C₂O₄)₅(H₂O)₄],
 and
 MM'[Zr(C₂O₄)₃]·xH₂O
 with M and M' = Ammonium, Alkali Metal, and Hydroxonium Ion
 H₂ₙ₊₁O <sub> n </sub>⁺ (n = 2,
 3, 4).
;
_journal_issue                   33
_journal_name_full               'ACS omega'
_journal_page_first              21260
_journal_page_last               21270
_journal_paper_doi               10.1021/acsomega.0c03224
_journal_volume                  5
_journal_year                    2020
_chemical_formula_sum            'C10 H30 O34 Zr2'
_chemical_formula_weight         876.78
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                78.421(2)
_cell_angle_beta                 86.155(2)
_cell_angle_gamma                89.945(2)
_cell_formula_units_Z            1
_cell_length_a                   6.9269(3)
_cell_length_b                   10.4427(6)
_cell_length_c                   10.6447(6)
_cell_measurement_reflns_used    3957
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.20
_cell_measurement_theta_min      2.50
_cell_volume                     752.56(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19393
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.943
_diffrn_reflns_theta_min         1.957
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.821
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.902
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.935
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             442
_exptl_crystal_size_max          0.258
_exptl_crystal_size_mid          0.152
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         2914
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0282
_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)+(0.0161P)²+0.6032P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0529
_refine_ls_wR_factor_ref         0.0566
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2498
_reflns_number_total             2914
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ao0c03224_si_002.cif
_cod_data_source_block           H2Zr2Ox5
_cod_depositor_comments
'Adding full bibliography for 4517899--4517905.cif.'
_cod_database_code               4517900
_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.
;
_shelxl_version_number           2013-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.31140(4) 0.84260(2) 0.83962(2) 0.01849(8) Uani 1 1 d . . . . .
C1 C 0.5600(3) 1.0368(2) 0.9418(2) 0.0200(6) Uani 1 1 d . . . . .
C2 C -0.0280(4) 0.9162(3) 0.6740(2) 0.0219(6) Uani 1 1 d . . . . .
C3 C 0.0144(4) 1.0390(3) 0.7266(2) 0.0229(6) Uani 1 1 d . . . . .
C4 C 0.4856(4) 0.5779(3) 0.8125(3) 0.0256(6) Uani 1 1 d . . . . .
C5 C 0.6370(4) 0.6460(3) 0.8770(3) 0.0250(6) Uani 1 1 d . . . . .
O1 O 0.4466(3) 0.9020(2) 0.64926(18) 0.0296(5) Uani 1 1 d D . . . .
H1 H 0.553(4) 0.936(3) 0.635(3) 0.035 Uiso 1 1 d D U . . .
H2 H 0.424(4) 0.861(3) 0.589(3) 0.035 Uiso 1 1 d D U . . .
O2 O 0.0825(3) 0.7335(2) 0.9620(2) 0.0336(5) Uani 1 1 d D . . . .
H3 H 0.006(4) 0.688(3) 0.938(3) 0.040 Uiso 1 1 d D U . . .
H4 H 0.089(4) 0.709(3) 1.042(3) 0.040 Uiso 1 1 d D U . . .
O3 O 0.3191(3) 0.88200(18) 1.03668(17) 0.0262(4) Uani 1 1 d . . . . .
O4 O 0.5277(2) 1.00969(17) 0.83624(16) 0.0237(4) Uani 1 1 d . . . . .
O5 O 0.1469(3) 1.02283(17) 0.80715(18) 0.0272(4) Uani 1 1 d . . . . .
O6 O 0.0829(2) 0.82109(17) 0.71125(17) 0.0251(4) Uani 1 1 d . . . . .
O7 O 0.3370(3) 0.64821(17) 0.78541(18) 0.0285(4) Uani 1 1 d . . . . .
O8 O 0.5789(3) 0.75479(18) 0.90301(19) 0.0327(5) Uani 1 1 d . . . . .
O9 O -0.1584(3) 0.91605(19) 0.60054(18) 0.0306(5) Uani 1 1 d . . . . .
O10 O -0.0717(3) 1.14060(18) 0.69051(19) 0.0320(5) Uani 1 1 d . . . . .
O11 O 0.7951(3) 0.5964(2) 0.8968(2) 0.0390(5) Uani 1 1 d . . . . .
O12 O 0.5141(3) 0.46793(19) 0.7922(2) 0.0381(5) Uani 1 1 d . . . . .
O13 O 1.0878(3) 0.5467(2) 0.6354(2) 0.0427(6) Uani 1 1 d D . . . .
H5 H 1.162(5) 0.589(3) 0.669(3) 0.051 Uiso 1 1 d D U . . .
H6 H 1.036(5) 0.478(3) 0.688(3) 0.051 Uiso 1 1 d D U . . .
H7 H 0.960(4) 0.608(3) 0.588(3) 0.051 Uiso 1 1 d D U . . .
O14 O 0.8189(3) 0.6772(2) 0.5470(2) 0.0437(6) Uani 1 1 d D . . . .
H8 H 0.826(5) 0.759(3) 0.562(3) 0.052 Uiso 1 1 d D U . . .
H9 H 0.792(5) 0.677(3) 0.475(3) 0.052 Uiso 1 1 d D U . . .
O15 O 0.6331(4) 0.2056(3) 0.5336(2) 0.0566(7) Uani 1 1 d D . . . .
H10 H 0.718(5) 0.164(4) 0.578(3) 0.068 Uiso 1 1 d D U . . .
H11 H 0.542(5) 0.226(4) 0.586(3) 0.068 Uiso 1 1 d D U . . .
O16 O 0.8873(3) 0.3610(2) 0.7889(2) 0.0320(5) Uani 1 1 d D . . . .
H12 H 0.888(4) 0.297(3) 0.756(3) 0.038 Uiso 1 1 d D U . . .
H13 H 0.781(4) 0.391(3) 0.791(3) 0.038 Uiso 1 1 d D U . . .
O17 O 0.3325(3) 0.2828(2) 0.6897(2) 0.0392(5) Uani 1 1 d D . . . .
H14 H 0.279(5) 0.226(3) 0.747(3) 0.047 Uiso 1 1 d D U . . .
H15 H 0.370(5) 0.342(3) 0.724(3) 0.047 Uiso 1 1 d D U . . .
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'
O O 0.0106 0.0060 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zr1 O2 147.72(7) . . ?
O1 Zr1 O8 89.42(8) . . ?
O2 Zr1 O8 106.52(8) . . ?
O1 Zr1 O5 88.45(7) . . ?
O2 Zr1 O5 93.42(8) . . ?
O8 Zr1 O5 144.89(7) . . ?
O1 Zr1 O6 75.32(7) . . ?
O2 Zr1 O6 74.71(7) . . ?
O8 Zr1 O6 140.70(7) . . ?
O5 Zr1 O6 71.87(6) . . ?
O1 Zr1 O3 141.40(7) . . ?
O2 Zr1 O3 70.62(7) . . ?
O8 Zr1 O3 77.09(7) . . ?
O5 Zr1 O3 82.99(7) . . ?
O6 Zr1 O3 135.40(7) . . ?
O1 Zr1 O7 80.74(7) . . ?
O2 Zr1 O7 78.42(8) . . ?
O8 Zr1 O7 70.95(6) . . ?
O5 Zr1 O7 142.80(6) . . ?
O6 Zr1 O7 70.96(6) . . ?
O3 Zr1 O7 126.19(7) . . ?
O1 Zr1 O4 70.55(7) . . ?
O2 Zr1 O4 140.55(7) . . ?
O8 Zr1 O4 72.83(7) . . ?
O5 Zr1 O4 73.45(6) . . ?
O6 Zr1 O4 131.26(6) . . ?
O3 Zr1 O4 70.93(6) . . ?
O7 Zr1 O4 133.41(7) . . ?
O4 C1 O3 127.7(2) . 2_677 ?
O4 C1 C1 116.4(3) . 2_677 ?
O3 C1 C1 115.9(3) 2_677 2_677 ?
O9 C2 O6 125.4(2) . . ?
O9 C2 C3 120.4(2) . . ?
O6 C2 C3 114.2(2) . . ?
O10 C3 O5 125.7(2) . . ?
O10 C3 C2 120.8(2) . . ?
O5 C3 C2 113.5(2) . . ?
O12 C4 O7 126.8(2) . . ?
O12 C4 C5 120.4(2) . . ?
O7 C4 C5 112.8(2) . . ?
O11 C5 O8 126.7(2) . . ?
O11 C5 C4 120.2(2) . . ?
O8 C5 C4 113.1(2) . . ?
C1 O3 Zr1 119.38(16) 2_677 . ?
C1 O4 Zr1 116.91(16) . . ?
C3 O5 Zr1 120.20(16) . . ?
C2 O6 Zr1 119.83(15) . . ?
C4 O7 Zr1 120.32(15) . . ?
C5 O8 Zr1 122.41(16) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 O1 2.147(2) . ?
Zr1 O2 2.154(2) . ?
Zr1 O8 2.1555(18) . ?
Zr1 O5 2.1789(18) . ?
Zr1 O6 2.1994(16) . ?
Zr1 O3 2.2212(17) . ?
Zr1 O7 2.2228(18) . ?
Zr1 O4 2.2940(17) . ?
C1 O4 1.247(3) . ?
C1 O3 1.256(3) 2_677 ?
C1 C1 1.516(5) 2_677 ?
C2 O9 1.234(3) . ?
C2 O6 1.271(3) . ?
C2 C3 1.534(4) . ?
C3 O10 1.223(3) . ?
C3 O5 1.286(3) . ?
C4 O12 1.224(3) . ?
C4 O7 1.279(3) . ?
C4 C5 1.540(4) . ?
C5 O11 1.223(3) . ?
C5 O8 1.280(3) . ?
O3 C1 1.256(3) 2_677 ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168346747
