#------------------------------------------------------------------------------
#$Date: 2020-09-04 03:28:54 +0300 (Fri, 04 Sep 2020) $
#$Revision: 255860 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/79/4517904.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_4517904
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 H7 O15 Rb Zr'
_chemical_formula_weight         495.81
_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                79.179(3)
_cell_angle_beta                 72.476(4)
_cell_angle_gamma                76.975(3)
_cell_formula_units_Z            2
_cell_length_a                   7.7027(5)
_cell_length_b                   8.9788(6)
_cell_length_c                   10.6518(7)
_cell_measurement_reflns_used    3200
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.87
_cell_measurement_theta_min      2.80
_cell_volume                     678.70(8)
_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 0.766
_diffrn_measured_fraction_theta_max 0.995
_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  0.0655
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 0.766
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            14524
_diffrn_reflns_point_group_measured_fraction_full 0.766
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         22.999
_diffrn_reflns_theta_min         2.348
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    4.459
_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    2.426
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.902
_refine_diff_density_min         -0.987
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         1886
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0440P)²+3.9128P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.0986
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1537
_reflns_number_total             1886
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ao0c03224_si_002.cif
_cod_data_source_block           RbHZrOx
_cod_depositor_comments
'Adding full bibliography for 4517899--4517905.cif.'
_cod_database_code               4517904
_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 0.24642(8) 0.61141(7) 0.74627(6) 0.0149(2) Uani 1 1 d . . . . .
Rb1 Rb 0.49609(16) 1.13991(11) 0.81091(9) 0.0666(4) Uani 1 1 d . . . . .
C1 C -0.0420(9) 0.8622(8) 0.6479(7) 0.0257(16) Uani 1 1 d . . . . .
C2 C -0.0724(10) 0.7080(8) 0.6224(7) 0.0282(17) Uani 1 1 d . . . . .
C3 C -0.0383(8) 0.5830(7) 1.0138(6) 0.0175(15) Uani 1 1 d . . . . .
C4 C 0.4963(9) 0.7300(8) 0.8614(7) 0.0258(16) Uani 1 1 d . . . . .
C5 C 0.5199(9) 0.5809(7) 0.4757(6) 0.0173(14) Uani 1 1 d . . . . .
C6 C 0.5823(10) 0.5590(8) 0.8518(7) 0.0270(17) Uani 1 1 d . . . . .
O1 O 0.1585(6) 0.4008(5) 0.8773(4) 0.0210(10) Uani 1 1 d . . . . .
O2 O 0.1087(6) 0.8461(5) 0.6839(4) 0.0220(10) Uani 1 1 d . . . . .
O3 O 0.3587(6) 0.7742(5) 0.8094(5) 0.0265(11) Uani 1 1 d . . . . .
O4 O 0.3627(6) 1.4007(5) 0.6328(4) 0.0202(10) Uani 1 1 d . . . . .
O5 O 0.4263(6) 0.6829(5) 0.5492(4) 0.0212(10) Uani 1 1 d . . . . .
O6 O 0.0273(6) 0.6848(5) 0.9271(4) 0.0213(10) Uani 1 1 d . . . . .
O7 O 0.4934(6) 0.4912(5) 0.7996(5) 0.0260(11) Uani 1 1 d . . . . .
O8 O 0.0374(6) 0.5901(5) 0.6610(5) 0.0289(11) Uani 1 1 d . . . . .
O9 O 0.7168(6) 0.4961(6) 0.8929(5) 0.0359(13) Uani 1 1 d . . . . .
O10 O -0.1493(7) 0.9825(6) 0.6340(6) 0.0446(14) Uani 1 1 d . . . . .
O11 O 0.5581(8) 0.8097(6) 0.9122(6) 0.0450(15) Uani 1 1 d . . . . .
O12 O -0.1926(8) 0.7041(6) 0.5699(6) 0.0484(15) Uani 1 1 d . . . . .
O13 O 0.3487(8) 1.0550(6) 0.5697(6) 0.0409(14) Uani 1 1 d D . . . .
H1 H 0.5000 1.0000 0.5000 0.049 Uiso 1 2 d S U P . .
H2 H 0.282(10) 0.990(8) 0.580(9) 0.049 Uiso 1 1 d D U . . .
H3 H 0.301(11) 1.126(8) 0.519(7) 0.049 Uiso 1 1 d D U . . .
O14 O -0.0786(12) 1.2646(10) 0.7388(10) 0.105(3) Uani 1 1 d . . . . .
O15 O 0.0911(13) 1.0429(9) 0.8863(9) 0.116(4) Uani 1 1 d . . . . .
H4 H 0.0000 1.0000 1.0000 0.139 Uiso 1 2 d S U P . .
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'
Rb Rb -0.9393 2.9676 '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
O8 Zr1 O7 143.95(18) . . ?
O8 Zr1 O3 143.58(18) . . ?
O7 Zr1 O3 72.08(17) . . ?
O8 Zr1 O5 91.64(17) . . ?
O7 Zr1 O5 87.39(17) . . ?
O3 Zr1 O5 83.42(17) . . ?
O8 Zr1 O2 71.88(17) . . ?
O7 Zr1 O2 141.41(17) . . ?
O3 Zr1 O2 71.99(17) . . ?
O5 Zr1 O2 75.00(16) . . ?
O8 Zr1 O1 81.77(17) . . ?
O7 Zr1 O1 76.77(16) . . ?
O3 Zr1 O1 123.19(17) . . ?
O5 Zr1 O1 141.14(15) . . ?
O2 Zr1 O1 136.42(15) . . ?
O8 Zr1 O6 89.74(17) . . ?
O7 Zr1 O6 109.96(17) . . ?
O3 Zr1 O6 76.26(16) . . ?
O5 Zr1 O6 147.13(16) . . ?
O2 Zr1 O6 74.28(16) . . ?
O1 Zr1 O6 71.48(15) . . ?
O8 Zr1 O4 73.71(17) . 1_545 ?
O7 Zr1 O4 71.90(16) . 1_545 ?
O3 Zr1 O4 136.42(16) . 1_545 ?
O5 Zr1 O4 71.26(15) . 1_545 ?
O2 Zr1 O4 130.29(16) . 1_545 ?
O1 Zr1 O4 70.12(14) . 1_545 ?
O6 Zr1 O4 139.86(15) . 1_545 ?
O8 Zr1 Rb1 100.29(13) . 1_545 ?
O7 Zr1 Rb1 44.92(12) . 1_545 ?
O3 Zr1 Rb1 116.11(12) . 1_545 ?
O5 Zr1 Rb1 100.53(11) . 1_545 ?
O2 Zr1 Rb1 170.60(12) . 1_545 ?
O1 Zr1 Rb1 44.38(11) . 1_545 ?
O6 Zr1 Rb1 111.51(11) . 1_545 ?
O4 Zr1 Rb1 40.65(11) 1_545 1_545 ?
O4 Rb1 O11 152.26(14) . . ?
O4 Rb1 O11 117.31(14) . 2_677 ?
O11 Rb1 O11 85.34(16) . 2_677 ?
O4 Rb1 O10 103.53(13) . 1_655 ?
O11 Rb1 O10 71.25(16) . 1_655 ?
O11 Rb1 O10 125.55(15) 2_677 1_655 ?
O4 Rb1 O1 51.30(11) . 1_565 ?
O11 Rb1 O1 132.20(15) . 1_565 ?
O11 Rb1 O1 72.76(14) 2_677 1_565 ?
O10 Rb1 O1 154.54(13) 1_655 1_565 ?
O4 Rb1 O7 50.98(12) . 1_565 ?
O11 Rb1 O7 156.71(14) . 1_565 ?
O11 Rb1 O7 74.22(14) 2_677 1_565 ?
O10 Rb1 O7 111.75(14) 1_655 1_565 ?
O1 Rb1 O7 51.93(11) 1_565 1_565 ?
O4 Rb1 O15 87.6(2) . . ?
O11 Rb1 O15 75.3(2) . . ?
O11 Rb1 O15 91.5(2) 2_677 . ?
O10 Rb1 O15 126.19(17) 1_655 . ?
O1 Rb1 O15 63.70(16) 1_565 . ?
O7 Rb1 O15 115.54(17) 1_565 . ?
O4 Rb1 O13 63.36(13) . . ?
O11 Rb1 O13 89.08(14) . . ?
O11 Rb1 O13 152.21(15) 2_677 . ?
O10 Rb1 O13 77.58(15) 1_655 . ?
O1 Rb1 O13 91.45(13) 1_565 . ?
O7 Rb1 O13 114.21(13) 1_565 . ?
O15 Rb1 O13 60.82(19) . . ?
O4 Rb1 O14 91.05(19) . 1_655 ?
O11 Rb1 O14 107.09(19) . 1_655 ?
O11 Rb1 O14 86.36(18) 2_677 1_655 ?
O10 Rb1 O14 57.18(16) 1_655 1_655 ?
O1 Rb1 O14 113.09(16) 1_565 1_655 ?
O7 Rb1 O14 61.33(16) 1_565 1_655 ?
O15 Rb1 O14 176.59(18) . 1_655 ?
O13 Rb1 O14 121.23(18) . 1_655 ?
O4 Rb1 C5 18.78(13) . 2_676 ?
O11 Rb1 C5 145.70(15) . 2_676 ?
O11 Rb1 C5 128.95(15) 2_677 2_676 ?
O10 Rb1 C5 85.03(15) 1_655 2_676 ?
O1 Rb1 C5 69.60(13) 1_565 2_676 ?
O7 Rb1 C5 55.58(14) 1_565 2_676 ?
O15 Rb1 C5 101.3(2) . 2_676 ?
O13 Rb1 C5 61.19(14) . 2_676 ?
O14 Rb1 C5 78.2(2) 1_655 2_676 ?
O4 Rb1 C4 134.40(15) . . ?
O11 Rb1 C4 17.88(15) . . ?
O11 Rb1 C4 99.64(16) 2_677 . ?
O10 Rb1 C4 71.22(15) 1_655 . ?
O1 Rb1 C4 127.27(14) 1_565 . ?
O7 Rb1 C4 173.84(14) 1_565 . ?
O15 Rb1 C4 64.48(19) . . ?
O13 Rb1 C4 71.46(15) . . ?
O14 Rb1 C4 118.47(18) 1_655 . ?
C5 Rb1 C4 130.55(15) 2_676 . ?
O4 Rb1 Zr1 30.80(8) . 1_565 ?
O11 Rb1 Zr1 162.66(12) . 1_565 ?
O11 Rb1 Zr1 86.54(11) 2_677 1_565 ?
O10 Rb1 Zr1 125.62(11) 1_655 1_565 ?
O1 Rb1 Zr1 30.46(8) 1_565 1_565 ?
O7 Rb1 Zr1 28.95(8) 1_565 1_565 ?
O15 Rb1 Zr1 89.62(16) . 1_565 ?
O13 Rb1 Zr1 90.99(10) . 1_565 ?
O14 Rb1 Zr1 87.64(15) 1_655 1_565 ?
C5 Rb1 Zr1 44.97(10) 2_676 1_565 ?
C4 Rb1 Zr1 153.34(12) . 1_565 ?
O10 C1 O2 126.0(7) . . ?
O10 C1 C2 122.2(7) . . ?
O2 C1 C2 111.9(6) . . ?
O12 C2 O8 125.3(7) . . ?
O12 C2 C1 120.9(7) . . ?
O8 C2 C1 113.7(6) . . ?
O6 C3 O1 128.3(6) . 2_567 ?
O6 C3 C3 116.3(7) . 2_567 ?
O1 C3 C3 115.3(7) 2_567 2_567 ?
O11 C4 O3 126.4(7) . . ?
O11 C4 C6 121.3(6) . . ?
O3 C4 C6 112.3(6) . . ?
O11 C4 Rb1 47.8(4) . . ?
O3 C4 Rb1 82.2(4) . . ?
C6 C4 Rb1 155.6(4) . . ?
O4 C5 O5 127.3(6) 2_676 . ?
O4 C5 C5 116.6(7) 2_676 2_666 ?
O5 C5 C5 116.0(7) . 2_666 ?
O4 C5 Rb1 49.2(3) 2_676 2_676 ?
O5 C5 Rb1 89.5(4) . 2_676 ?
C5 C5 Rb1 137.2(5) 2_666 2_676 ?
O9 C6 O7 125.2(7) . . ?
O9 C6 C4 122.3(6) . . ?
O7 C6 C4 112.5(6) . . ?
C3 O1 Zr1 118.6(4) 2_567 . ?
C3 O1 Rb1 128.6(4) 2_567 1_545 ?
Zr1 O1 Rb1 105.16(14) . 1_545 ?
C1 O2 Zr1 118.9(4) . . ?
C4 O3 Zr1 121.2(4) . . ?
C5 O4 Zr1 116.4(4) 2_676 1_565 ?
C5 O4 Rb1 112.0(4) 2_676 . ?
Zr1 O4 Rb1 108.55(15) 1_565 . ?
C5 O5 Zr1 119.0(4) . . ?
C3 O6 Zr1 118.3(4) . . ?
C6 O7 Zr1 121.2(4) . . ?
C6 O7 Rb1 129.9(4) . 1_545 ?
Zr1 O7 Rb1 106.13(16) . 1_545 ?
C2 O8 Zr1 122.0(5) . . ?
C1 O10 Rb1 134.2(5) . 1_455 ?
C4 O11 Rb1 114.3(5) . . ?
C4 O11 Rb1 133.9(5) . 2_677 ?
Rb1 O11 Rb1 94.66(16) . 2_677 ?
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 O8 2.130(5) . ?
Zr1 O7 2.145(5) . ?
Zr1 O3 2.151(5) . ?
Zr1 O5 2.209(4) . ?
Zr1 O2 2.213(4) . ?
Zr1 O1 2.236(4) . ?
Zr1 O6 2.239(4) . ?
Zr1 O4 2.299(4) 1_545 ?
Zr1 Rb1 4.2577(11) 1_545 ?
Rb1 O4 2.926(4) . ?
Rb1 O11 2.942(5) . ?
Rb1 O11 2.958(6) 2_677 ?
Rb1 O10 3.028(5) 1_655 ?
Rb1 O1 3.085(4) 1_565 ?
Rb1 O7 3.130(5) 1_565 ?
Rb1 O15 3.254(10) . ?
Rb1 O13 3.369(6) . ?
Rb1 O14 3.520(9) 1_655 ?
Rb1 C5 3.582(6) 2_676 ?
Rb1 C4 3.618(7) . ?
Rb1 Zr1 4.2577(11) 1_565 ?
C1 O10 1.219(8) . ?
C1 O2 1.298(8) . ?
C1 C2 1.540(10) . ?
C2 O12 1.227(9) . ?
C2 O8 1.284(8) . ?
C3 O6 1.247(7) . ?
C3 O1 1.257(7) 2_567 ?
C3 C3 1.523(13) 2_567 ?
C4 O11 1.219(8) . ?
C4 O3 1.292(8) . ?
C4 C6 1.538(10) . ?
C5 O4 1.244(7) 2_676 ?
C5 O5 1.266(7) . ?
C5 C5 1.515(13) 2_666 ?
C5 Rb1 3.582(6) 2_676 ?
C6 O9 1.225(9) . ?
C6 O7 1.300(8) . ?
O1 C3 1.257(7) 2_567 ?
O1 Rb1 3.085(4) 1_545 ?
O4 C5 1.244(7) 2_676 ?
O4 Zr1 2.299(4) 1_565 ?
O7 Rb1 3.130(5) 1_545 ?
O10 Rb1 3.028(5) 1_455 ?
O11 Rb1 2.958(6) 2_677 ?
O14 Rb1 3.520(9) 1_455 ?
