Zirconium Oxalates: Zr(OH)<sub>2</sub>(C<sub>2</sub>O<sub>4</sub>), (H<sub>11</sub>O<sub>5</sub>)<sub>2</sub>[Zr<sub>2</sub>(C<sub>2</sub>O<sub>4</sub>)<sub>5</sub>(H<sub>2</sub>O)<sub>4</sub>], and MM'[Zr(C<sub>2</sub>O<sub>4</sub>)<sub>3</sub>]·<i>x</i>H<sub>2</sub>O with M and M' = Ammonium, Alkali Metal, and Hydroxonium Ion H<sub>2<i>n</i>+1</sub>O <sub> <i>n</i> </sub><sup>+</sup> (<i>n</i> = 2, 3, 4).
Thomas, Rudy; Devaux, Philippe; Rivenet, Murielle; Henry, Natacha; Abraham, Francis; ACS omega 5 (2020) 21260–21270; doi:10.1021/acsomega.0c03224

data_4517903
_publ_section_title
;
 Zirconium Oxalates: Zr(OH)<sub>2</sub>(C<sub>2</sub>O<sub>4</sub>),
 (H<sub>11</sub>O<sub>5</sub>)<sub>2</sub>[Zr<sub>2</sub>(C<sub>2</sub>O<sub>4</sub>)<sub>5</sub>(H<sub>2</sub>O)<sub>4</sub>],
 and
 MM'[Zr(C<sub>2</sub>O<sub>4</sub>)<sub>3</sub>]&#x00B7;<i>x</i>H<sub>2</sub>O
 with M and M' = Ammonium, Alkali Metal, and Hydroxonium Ion
 H<sub>2<i>n</i>+1</sub>O <sub> <i>n</i> </sub><sup>+</sup> (<i>n</i> = 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            'C6 H13 N O16 Zr'
_chemical_formula_weight         446.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 107.699(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3411(7)
_cell_length_b                   11.1701(8)
_cell_length_c                   14.2537(9)
_cell_measurement_reflns_used    1543
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.20
_cell_measurement_theta_min      3.2
_cell_volume                     1416.85(17)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0446
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            58123
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.669
_diffrn_reflns_theta_min         2.361
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.871
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.800
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.093
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.295
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.053
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         5638
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0248
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0272P)^2^+0.7459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0583
_refine_ls_wR_factor_ref         0.0624
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4715
_reflns_number_total             5638
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao0c03224_si_002.cif
_cod_data_source_block           NH4HZrOx3
_cod_depositor_comments
'Adding full bibliography for 4517899--4517905.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4517903
_shelxl_version_number           2013-3
_shelx_res_checksum              23093
_shelx_hkl_checksum              43942