#------------------------------------------------------------------------------
#$Date: 2020-09-04 03:28:54 +0300 (Fri, 04 Sep 2020) $
#$Revision: 255860 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/79/4517902.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_4517902
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            'C6 H9 K O16 Zr'
_chemical_formula_weight         467.45
_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                 107.718(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2166(9)
_cell_length_b                   11.1690(10)
_cell_length_c                   14.0940(15)
_cell_measurement_reflns_used    4190
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.83
_cell_measurement_theta_min      2.95
_cell_volume                     1382.0(2)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0570
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21953
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.527
_diffrn_reflns_theta_min         2.320
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.191
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.885
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.247
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         2868
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0291
_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)+(0.0249P)²+0.5987P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0593
_refine_ls_wR_factor_ref         0.0640
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2299
_reflns_number_total             2868
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ao0c03224_si_002.cif
_cod_data_source_block           KHZrOx3
_cod_depositor_comments
'Adding full bibliography for 4517899--4517905.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4517902
_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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 0.39097(3) 0.09841(2) 0.24535(2) 0.01209(9) Uani 1 1 d . . . . .
K1 K 0.07195(8) 0.47019(7) 0.13247(5) 0.03542(19) Uani 1 1 d . . . . .
C1 C 0.4208(3) 0.3700(2) 0.23739(19) 0.0158(6) Uani 1 1 d . . . . .
C2 C 0.4174(3) -0.1742(2) 0.24478(18) 0.0150(6) Uani 1 1 d . . . . .
C3 C 0.2893(4) 0.1080(2) 0.0195(2) 0.0228(7) Uani 1 1 d . . . . .
C4 C 0.1396(4) 0.1148(2) 0.0459(2) 0.0219(7) Uani 1 1 d . . . . .
C5 C 0.2746(3) 0.1063(2) 0.4248(2) 0.0193(6) Uani 1 1 d . . . . .
C6 C 0.4461(3) 0.1306(2) 0.4672(2) 0.0193(6) Uani 1 1 d . . . . .
O1 O 0.3185(2) -0.09281(15) 0.23085(14) 0.0190(4) Uani 1 1 d . . . . .
O2 O 0.4014(2) 0.48090(15) 0.23263(13) 0.0186(4) Uani 1 1 d . . . . .
O3 O 0.3987(2) -0.28402(15) 0.24571(13) 0.0174(4) Uani 1 1 d . . . . .
O4 O 0.3204(2) 0.29093(15) 0.22829(14) 0.0189(4) Uani 1 1 d . . . . .
O5 O 0.2921(3) 0.11826(19) -0.06598(15) 0.0353(6) Uani 1 1 d . . . . .
O6 O 0.0183(3) 0.13229(19) -0.01775(16) 0.0350(5) Uani 1 1 d . . . . .
O7 O 0.4074(2) 0.09151(16) 0.09702(14) 0.0213(4) Uani 1 1 d . . . . .
O8 O 0.1594(2) 0.10142(16) 0.14017(13) 0.0195(4) Uani 1 1 d . . . . .
O9 O 0.5136(2) 0.13160(17) 0.39896(14) 0.0231(5) Uani 1 1 d . . . . .
O10 O 0.2324(2) 0.08923(16) 0.32972(14) 0.0216(4) Uani 1 1 d . . . . .
O11 O 0.5094(2) 0.14762(19) 0.55511(14) 0.0298(5) Uani 1 1 d . . . . .
O12 O 0.1929(3) 0.10343(18) 0.47785(15) 0.0321(5) Uani 1 1 d . . . . .
O13 O 0.0821(3) 0.6338(2) 0.29903(18) 0.0339(6) Uani 1 1 d D . . . .
H1 H 0.193(3) 0.636(3) 0.368(2) 0.041 Uiso 1 1 d D U . . .
H2 H 0.011(4) 0.612(3) 0.317(3) 0.041 Uiso 1 1 d D U . . .
H3 H 0.060(4) 0.701(3) 0.266(2) 0.041 Uiso 1 1 d D U . . .
O14 O -0.0139(3) 0.3414(2) 0.27719(17) 0.0371(6) Uani 1 1 d D . . . .
H4 H 0.058(4) 0.340(3) 0.329(2) 0.044 Uiso 1 1 d D U . . .
H5 H -0.088(4) 0.367(3) 0.288(3) 0.044 Uiso 1 1 d D U . . .
O15 O 0.3171(3) 0.6471(2) 0.43946(18) 0.0332(5) Uani 1 1 d D . . . .
H6 H 0.385(4) 0.608(3) 0.428(3) 0.040 Uiso 1 1 d D U . . .
H7 H 0.355(4) 0.717(2) 0.446(2) 0.040 Uiso 1 1 d D U . . .
O16 O -0.1474(3) 0.3472(2) -0.0197(2) 0.0458(7) Uani 1 1 d D . . . .
H8 H -0.115(4) 0.280(3) -0.029(3) 0.055 Uiso 1 1 d D U . . .
H9 H -0.237(3) 0.351(4) -0.044(3) 0.055 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'
H H 0.0000 0.0000 '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
O7 Zr1 O9 144.86(8) . . ?
O7 Zr1 O10 143.14(7) . . ?
O9 Zr1 O10 71.84(7) . . ?
O7 Zr1 O8 71.64(7) . . ?
O9 Zr1 O8 141.50(7) . . ?
O10 Zr1 O8 71.91(7) . . ?
O7 Zr1 O1 89.10(7) . . ?
O9 Zr1 O1 107.99(7) . . ?
O10 Zr1 O1 76.69(7) . . ?
O8 Zr1 O1 75.55(7) . . ?
O7 Zr1 O4 91.96(7) . . ?
O9 Zr1 O4 89.37(7) . . ?
O10 Zr1 O4 83.17(7) . . ?
O8 Zr1 O4 73.86(7) . . ?
O1 Zr1 O4 147.34(7) . . ?
O7 Zr1 O2 78.76(7) . 2_645 ?
O9 Zr1 O2 78.35(7) . 2_645 ?
O10 Zr1 O2 125.83(7) . 2_645 ?
O8 Zr1 O2 135.13(6) . 2_645 ?
O1 Zr1 O2 70.96(6) . 2_645 ?
O4 Zr1 O2 141.08(7) . 2_645 ?
O7 Zr1 O3 76.50(7) . 2_655 ?
O9 Zr1 O3 70.84(7) . 2_655 ?
O10 Zr1 O3 134.17(6) . 2_655 ?
O8 Zr1 O3 130.85(6) . 2_655 ?
O1 Zr1 O3 140.52(6) . 2_655 ?
O4 Zr1 O3 70.83(6) . 2_655 ?
O2 Zr1 O3 70.25(6) 2_645 2_655 ?
O14 K1 O16 164.11(8) . 3_565 ?
O14 K1 O16 90.43(8) . . ?
O16 K1 O16 99.66(7) 3_565 . ?
O14 K1 O12 132.14(7) . 4_565 ?
O16 K1 O12 63.53(7) 3_565 4_565 ?
O16 K1 O12 68.59(7) . 4_565 ?
O14 K1 O12 106.15(7) . 2 ?
O16 K1 O12 68.48(7) 3_565 2 ?
O16 K1 O12 63.03(7) . 2 ?
O12 K1 O12 101.57(6) 4_565 2 ?
O14 K1 O2 98.68(7) . . ?
O16 K1 O2 81.02(7) 3_565 . ?
O16 K1 O2 141.60(7) . . ?
O12 K1 O2 77.98(6) 4_565 . ?
O12 K1 O2 145.28(6) 2 . ?
O14 K1 O13 71.73(7) . . ?
O16 K1 O13 92.71(8) 3_565 . ?
O16 K1 O13 138.46(8) . . ?
O12 K1 O13 149.29(7) 4_565 . ?
O12 K1 O13 85.76(7) 2 . ?
O2 K1 O13 79.32(6) . . ?
O14 K1 O4 71.27(6) . . ?
O16 K1 O4 116.69(7) 3_565 . ?
O16 K1 O4 106.68(7) . . ?
O12 K1 O4 74.47(6) 4_565 . ?
O12 K1 O4 169.61(6) 2 . ?
O2 K1 O4 44.13(5) . . ?
O13 K1 O4 102.56(6) . . ?
O14 K1 O10 69.25(6) . 2 ?
O16 K1 O10 99.73(6) 3_565 2 ?
O16 K1 O10 82.56(7) . 2 ?
O12 K1 O10 142.21(6) 4_565 2 ?
O12 K1 O10 41.75(5) 2 2 ?
O2 K1 O10 135.53(5) . 2 ?
O13 K1 O10 56.21(6) . 2 ?
O4 K1 O10 139.47(5) . 2 ?
O14 K1 C1 87.25(7) . . ?
O16 K1 C1 97.18(7) 3_565 . ?
O16 K1 C1 123.48(7) . . ?
O12 K1 C1 71.98(6) 4_565 . ?
O12 K1 C1 165.56(7) 2 . ?
O2 K1 C1 22.17(6) . . ?
O13 K1 C1 93.60(7) . . ?
O4 K1 C1 22.39(5) . . ?
O10 K1 C1 145.79(6) 2 . ?
O14 K1 C5 87.10(7) . 2 ?
O16 K1 C5 85.27(7) 3_565 2 ?
O16 K1 C5 68.47(7) . 2 ?
O12 K1 C5 120.25(7) 4_565 2 ?
O12 K1 C5 20.09(6) 2 2 ?
O2 K1 C5 148.67(6) . 2 ?
O13 K1 C5 73.31(7) . 2 ?
O4 K1 C5 157.99(6) . 2 ?
O10 K1 C5 22.14(5) 2 2 ?
C1 K1 C5 166.82(7) . 2 ?
O14 K1 K1 138.52(6) . 3_565 ?
O16 K1 K1 50.02(6) 3_565 3_565 ?
O16 K1 K1 49.63(6) . 3_565 ?
O12 K1 K1 51.07(5) 4_565 3_565 ?
O12 K1 K1 50.50(4) 2 3_565 ?
O2 K1 K1 119.25(5) . 3_565 ?
O13 K1 K1 128.20(6) . 3_565 ?
O4 K1 K1 124.76(5) . 3_565 ?
O10 K1 K1 91.72(4) 2 3_565 ?
C1 K1 K1 121.69(5) . 3_565 ?
C5 K1 K1 69.58(5) 2 3_565 ?
O2 C1 O4 127.0(3) . . ?
O2 C1 C2 116.6(2) . 2_655 ?
O4 C1 C2 116.4(2) . 2_655 ?
O2 C1 K1 62.37(14) . . ?
O4 C1 K1 66.79(14) . . ?
C2 C1 K1 163.59(16) 2_655 . ?
O3 C2 O1 128.2(2) . . ?
O3 C2 C1 116.9(2) . 2_645 ?
O1 C2 C1 114.8(2) . 2_645 ?
O5 C3 O7 125.5(3) . . ?
O5 C3 C4 121.7(3) . . ?
O7 C3 C4 112.8(2) . . ?
O6 C4 O8 125.9(3) . . ?
O6 C4 C3 121.4(3) . . ?
O8 C4 C3 112.8(3) . . ?
O12 C5 O10 126.1(3) . . ?
O12 C5 C6 121.6(3) . . ?
O10 C5 C6 112.3(2) . . ?
O12 C5 K1 54.59(15) . 2_545 ?
O10 C5 K1 73.96(15) . 2_545 ?
C6 C5 K1 162.22(17) . 2_545 ?
O11 C6 O9 124.6(3) . . ?
O11 C6 C5 122.9(3) . . ?
O9 C6 C5 112.5(2) . . ?
C2 O1 Zr1 119.65(16) . . ?
C1 O2 Zr1 117.81(17) . 2_655 ?
C1 O2 K1 95.46(16) . . ?
Zr1 O2 K1 142.88(7) 2_655 . ?
C2 O3 Zr1 116.42(16) . 2_645 ?
C1 O4 Zr1 118.89(17) . . ?
C1 O4 K1 90.82(15) . . ?
Zr1 O4 K1 146.88(8) . . ?
C3 O7 Zr1 121.68(18) . . ?
C4 O8 Zr1 119.91(18) . . ?
C6 O9 Zr1 121.52(17) . . ?
C5 O10 Zr1 121.80(17) . . ?
C5 O10 K1 83.90(15) . 2_545 ?
Zr1 O10 K1 149.95(8) . 2_545 ?
C5 O12 K1 159.8(2) . 4_566 ?
C5 O12 K1 105.32(18) . 2_545 ?
K1 O12 K1 78.43(6) 4_566 2_545 ?
K1 O16 K1 80.34(7) 3_565 . ?
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 O7 2.1429(18) . ?
Zr1 O9 2.1477(19) . ?
Zr1 O10 2.1486(18) . ?
Zr1 O8 2.1975(19) . ?
Zr1 O1 2.2284(17) . ?
Zr1 O4 2.2380(17) . ?
Zr1 O2 2.2623(18) 2_645 ?
Zr1 O3 2.3132(17) 2_655 ?
K1 O14 2.800(3) . ?
K1 O16 2.801(3) 3_565 ?
K1 O16 2.817(3) . ?
K1 O12 2.854(2) 4_565 ?
K1 O12 2.877(2) 2 ?
K1 O2 2.9361(19) . ?
K1 O13 2.954(3) . ?
K1 O4 3.0324(19) . ?
K1 O10 3.291(2) 2 ?
K1 C1 3.299(3) . ?
K1 C5 3.405(3) 2 ?
K1 K1 3.6237(14) 3_565 ?
C1 O2 1.251(3) . ?
C1 O4 1.257(3) . ?
C1 C2 1.517(4) 2_655 ?
C2 O3 1.240(3) . ?
C2 O1 1.259(3) . ?
C2 C1 1.517(4) 2_645 ?
C3 O5 1.218(3) . ?
C3 O7 1.299(4) . ?
C3 C4 1.536(4) . ?
C4 O6 1.217(3) . ?
C4 O8 1.294(3) . ?
C5 O12 1.213(3) . ?
C5 O10 1.291(3) . ?
C5 C6 1.535(4) . ?
C5 K1 3.405(3) 2_545 ?
C6 O11 1.214(3) . ?
C6 O9 1.294(3) . ?
O2 Zr1 2.2623(18) 2_655 ?
O3 Zr1 2.3132(17) 2_645 ?
O10 K1 3.291(2) 2_545 ?
O12 K1 2.854(2) 4_566 ?
O12 K1 2.878(2) 2_545 ?
O16 K1 2.801(3) 3_565 ?
