#------------------------------------------------------------------------------
#$Date: 2020-09-04 03:28:54 +0300 (Fri, 04 Sep 2020) $
#$Revision: 255860 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/79/4517903.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_4517903
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 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/[σ²(Fo²)+(0.0272P)²+0.7459P] where P=(Fo²+2Fc²)/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 > 2σ(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
_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 0.39207(2) 0.10223(2) 0.24528(2) 0.01235(4) Uani 1 1 d . . . . .
C1 C 0.42248(15) 0.37367(11) 0.23720(10) 0.0157(2) Uani 1 1 d . . . . .
C2 C 0.41857(14) -0.17082(11) 0.24606(9) 0.0150(2) Uani 1 1 d . . . . .
C3 C 0.29194(18) 0.10865(13) 0.02159(11) 0.0228(3) Uani 1 1 d . . . . .
C4 C 0.14367(17) 0.11696(13) 0.04747(11) 0.0226(3) Uani 1 1 d . . . . .
C5 C 0.27927(17) 0.10932(13) 0.42349(11) 0.0205(2) Uani 1 1 d . . . . .
C6 C 0.44913(17) 0.13243(13) 0.46491(11) 0.0201(3) Uani 1 1 d . . . . .
O1 O 0.31977(11) -0.08951(8) 0.23237(8) 0.01972(19) Uani 1 1 d . . . . .
O2 O 0.40403(11) 0.48481(9) 0.23322(8) 0.0202(2) Uani 1 1 d . . . . .
O3 O 0.40000(11) -0.28038(8) 0.24682(8) 0.01835(18) Uani 1 1 d . . . . .
O4 O 0.32365(11) 0.29456(8) 0.22876(8) 0.01943(19) Uani 1 1 d . . . . .
O5 O 0.29344(17) 0.11701(13) -0.06305(9) 0.0374(3) Uani 1 1 d . . . . .
O6 O 0.02365(15) 0.13350(13) -0.01532(9) 0.0365(3) Uani 1 1 d . . . . .
O7 O 0.40804(12) 0.09391(10) 0.09894(8) 0.0227(2) Uani 1 1 d . . . . .
O8 O 0.16289(11) 0.10529(9) 0.14101(8) 0.02079(19) Uani 1 1 d . . . . .
O9 O 0.51530(12) 0.13449(11) 0.39731(8) 0.0232(2) Uani 1 1 d . . . . .
O10 O 0.23641(12) 0.09427(10) 0.32897(8) 0.0224(2) Uani 1 1 d . . . . .
O11 O 0.51191(14) 0.14733(12) 0.55260(8) 0.0310(3) Uani 1 1 d . . . . .
O12 O 0.19912(15) 0.10700(12) 0.47640(10) 0.0344(3) Uani 1 1 d . . . . .
O13 O 0.92280(15) 0.13622(14) 0.19831(11) 0.0362(3) Uani 1 1 d D . . . .
H1 H 0.812(2) 0.142(2) 0.1305(16) 0.043 Uiso 1 1 d D U . . .
H2 H 0.995(3) 0.120(2) 0.1795(18) 0.043 Uiso 1 1 d D U . . .
H3 H 0.945(3) 0.203(2) 0.2364(17) 0.043 Uiso 1 1 d D U . . .
O14 O 0.97917(18) 0.33935(15) 0.28315(10) 0.0404(3) Uani 1 1 d D . . . .
H4 H 1.045(3) 0.341(2) 0.3306(17) 0.048 Uiso 1 1 d D U . . .
H5 H 0.895(3) 0.366(2) 0.2913(19) 0.048 Uiso 1 1 d D U . . .
O15 O 0.68493(15) 0.14667(13) 0.06360(11) 0.0340(3) Uani 1 1 d D . . . .
H6 H 0.621(3) 0.105(2) 0.0791(18) 0.041 Uiso 1 1 d D U . . .
H7 H 0.647(3) 0.213(2) 0.0616(18) 0.041 Uiso 1 1 d D U . . .
O16 O 0.84180(17) 0.34126(15) 0.97184(14) 0.0488(4) Uani 1 1 d D . . . .
H8 H 0.870(3) 0.270(2) 0.967(2) 0.059 Uiso 1 1 d D U . . .
H9 H 0.745(3) 0.345(3) 0.947(2) 0.059 Uiso 1 1 d D U . . .
N1 N 0.0639(2) 0.46466(18) 0.12988(14) 0.0383(4) Uani 1 1 d D . . . .
H10 H -0.011(3) 0.424(2) 0.0850(18) 0.046 Uiso 1 1 d D U . . .
H11 H 0.055(3) 0.445(2) 0.1869(17) 0.046 Uiso 1 1 d D U . . .
H12 H 0.139(3) 0.430(2) 0.1215(18) 0.046 Uiso 1 1 d D U . . .
H13 H 0.067(3) 0.535(2) 0.1101(18) 0.046 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'
N N 0.0061 0.0033 '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
O7 Zr1 O10 143.23(4) . . ?
O7 Zr1 O9 144.57(4) . . ?
O10 Zr1 O9 72.09(4) . . ?
O7 Zr1 O8 71.60(4) . . ?
O10 Zr1 O8 72.06(4) . . ?
O9 Zr1 O8 142.06(4) . . ?
O7 Zr1 O4 92.38(4) . . ?
O10 Zr1 O4 82.98(4) . . ?
O9 Zr1 O4 89.63(4) . . ?
O8 Zr1 O4 74.09(4) . . ?
O7 Zr1 O1 89.25(4) . . ?
O10 Zr1 O1 76.54(4) . . ?
O9 Zr1 O1 107.39(4) . . ?
O8 Zr1 O1 75.66(4) . . ?
O4 Zr1 O1 147.45(4) . . ?
O7 Zr1 O2 78.51(4) . 2_645 ?
O10 Zr1 O2 125.99(4) . 2_645 ?
O9 Zr1 O2 77.85(4) . 2_645 ?
O8 Zr1 O2 135.04(4) . 2_645 ?
O4 Zr1 O2 140.94(4) . 2_645 ?
O1 Zr1 O2 71.07(4) . 2_645 ?
O7 Zr1 O3 76.46(4) . 2_655 ?
O10 Zr1 O3 134.13(4) . 2_655 ?
O9 Zr1 O3 70.89(4) . 2_655 ?
O8 Zr1 O3 130.68(4) . 2_655 ?
O4 Zr1 O3 70.71(3) . 2_655 ?
O1 Zr1 O3 140.67(4) . 2_655 ?
O2 Zr1 O3 70.23(4) 2_645 2_655 ?
O2 C1 O4 127.28(12) . . ?
O2 C1 C2 116.57(11) . 2_655 ?
O4 C1 C2 116.15(11) . 2_655 ?
O3 C2 O1 127.83(12) . . ?
O3 C2 C1 117.18(11) . 2_645 ?
O1 C2 C1 114.99(11) . 2_645 ?
O5 C3 O7 126.40(16) . . ?
O5 C3 C4 121.06(15) . . ?
O7 C3 C4 112.54(13) . . ?
O6 C4 O8 125.45(16) . . ?
O6 C4 C3 121.81(15) . . ?
O8 C4 C3 112.75(12) . . ?
O12 C5 O10 126.14(14) . . ?
O12 C5 C6 121.64(14) . . ?
O10 C5 C6 112.22(12) . . ?
O11 C6 O9 124.82(14) . . ?
O11 C6 C5 122.34(14) . . ?
O9 C6 C5 112.83(12) . . ?
C2 O1 Zr1 119.10(8) . . ?
C1 O2 Zr1 118.13(8) . 2_655 ?
C2 O3 Zr1 116.27(8) . 2_645 ?
C1 O4 Zr1 119.20(8) . . ?
C3 O7 Zr1 122.28(10) . . ?
C4 O8 Zr1 119.82(9) . . ?
C6 O9 Zr1 121.10(9) . . ?
C5 O10 Zr1 121.73(9) . . ?
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 2.1380(11) . ?
Zr1 O10 2.1448(11) . ?
Zr1 O9 2.1527(11) . ?
Zr1 O8 2.2042(10) . ?
Zr1 O4 2.2333(10) . ?
Zr1 O1 2.2365(10) . ?
Zr1 O2 2.2554(10) 2_645 ?
Zr1 O3 2.3176(10) 2_655 ?
C1 O2 1.2523(15) . ?
C1 O4 1.2570(16) . ?
C1 C2 1.5144(18) 2_655 ?
C2 O3 1.2365(15) . ?
C2 O1 1.2669(15) . ?
C2 C1 1.5143(18) 2_645 ?
C3 O5 1.2143(19) . ?
C3 O7 1.3007(18) . ?
C3 C4 1.541(2) . ?
C4 O6 1.2173(18) . ?
C4 O8 1.2967(18) . ?
C5 O12 1.2139(19) . ?
C5 O10 1.2944(18) . ?
C5 C6 1.537(2) . ?
C6 O11 1.2199(18) . ?
C6 O9 1.2935(18) . ?
O2 Zr1 2.2554(10) 2_655 ?
O3 Zr1 2.3176(10) 2_645 ?
