#------------------------------------------------------------------------------
#$Date: 2022-01-01 06:16:20 +0200 (Sat, 01 Jan 2022) $
#$Revision: 271664 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/10/89/2108901.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2108901
loop_
_publ_author_name
'Garkul, Ilia'
'Zadesenets, Andrey'
'Filatov, Evgeny'
'Baidina, Iraida'
'Tkachev, Sergey'
'Samsonenko, Denis'
'Korenev, Sergey'
_publ_section_title
;
Oxonium trans-bis(oxalato)rhodate and related sodium salts: a rare
example of crystalline complex acid
;
_journal_issue 6
_journal_name_full 'Acta Crystallographica Section B'
_journal_page_first 1048
_journal_page_last 1054
_journal_paper_doi 10.1107/S205252062101115X
_journal_volume 77
_journal_year 2021
_chemical_formula_moiety 'C4 H11 Na2 O14 Rh'
_chemical_formula_sum 'C4 H11 Na2 O14 Rh'
_chemical_formula_weight 432.02
_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
_atom_sites_solution_primary dual
_audit_creation_date 2021-06-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha 94.20(3)
_cell_angle_beta 99.40(3)
_cell_angle_gamma 98.10(3)
_cell_formula_units_Z 1
_cell_length_a 5.5500(11)
_cell_length_b 6.4400(13)
_cell_length_c 8.5900(17)
_cell_measurement_reflns_used 3338
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 31.52
_cell_measurement_theta_min 3.21
_cell_volume 298.42(11)
_computing_cell_refinement 'Bruker SAINT'
_computing_data_collection 'Bruker APEX2'
_computing_data_reduction 'Bruker SAINT'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature 150(2)
_diffrn_detector CCD
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type 'Bruker APEXII CCD area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device '\k-geometry diffractometer'
_diffrn_measurement_device_type 'Bruker APEX diffractometer'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0233
_diffrn_reflns_av_unetI/netI 0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -6
_diffrn_reflns_limit_l_max 9
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 3654
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 31.531
_diffrn_reflns_theta_min 2.415
_diffrn_source 'sealed tube'
_exptl_absorpt_coefficient_mu 1.585
_exptl_absorpt_correction_T_max 0.7462
_exptl_absorpt_correction_T_min 0.6611
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0409 before and 0.0312 after correction. The Ratio of minimum to maximum transmission is 0.8860. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour 'light yellow'
_exptl_crystal_colour_modifier light
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 2.404
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 214
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.12
_exptl_crystal_size_min 0.06
_refine_diff_density_max 0.814
_refine_diff_density_min -1.148
_refine_diff_density_rms 0.092
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.064
_refine_ls_hydrogen_treatment refxyz
_refine_ls_matrix_type full
_refine_ls_number_parameters 115
_refine_ls_number_reflns 1984
_refine_ls_number_restraints 6
_refine_ls_restrained_S_all 1.064
_refine_ls_R_factor_all 0.0172
_refine_ls_R_factor_gt 0.0170
_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/[\s^2^(Fo^2^)+0.2058P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0421
_refine_ls_wR_factor_ref 0.0426
_reflns_Friedel_coverage 0.000
_reflns_number_gt 1975
_reflns_number_total 1984
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file yh5016sup1.cif
_cod_data_source_block Na2Rh
_cod_database_code 2108901
_publcif_datablock.id {ffbded9b-fb91-462b-a3ca-93c3f3fc7256}
_shelx_shelxl_version_number 2017/1
_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.
;
_shelx_estimated_absorpt_t_max 0.911
_shelx_estimated_absorpt_t_min 0.742
_olex2_refinement_description
;
1. Fixed Uiso
At 1.5 times of:
All O(H,H) groups
2. Restrained distances
O2W-H2WA = O2W-H2WB
0.84 with sigma of 0.02
O3W-H3WA = O3W-H3WB
0.84 with sigma of 0.02
O1W-H1WA = O1W-H1W
0.84 with sigma of 0.02
3. Others
Fixed Sof: H1W(0.5)
;
_shelx_res_file
;
TITL my_a.res in P-1
n.res
created by SHELXL-2017/1 at 13:27:08 on 21-Jun-2021
REM Old TITL my in P1
REM SHELXT solution in P-1
REM R1 0.035, Rweak 0.054, Alpha 0.088, Orientation as input
REM Formula found by SHELXT: C4 O14 Na2 Rh
CELL 0.71073 5.55 6.44 8.59 94.2 99.4 98.1
ZERR 1 0.0011 0.0013 0.0017 0.03 0.03 0.03
LATT 1
SFAC C H Na O Rh
UNIT 4 11 2 14 1
DFIX 0.84 O2W H2Wa O2W H2Wb
DFIX 0.84 O3W H3Wa O3W H3Wb
DFIX 0.84 O1W H1Wa O1W H1W
L.S. 10
PLAN 10
SIZE 0.2 0.12 0.06
TEMP -123(2)
BOND $H
list 4
fmap 2 53
ACTA
MERG 2
OMIT 0 180
REM
REM
REM
WGHT 0.000000 0.205800
FVAR 1.00270
RH1 5 1.000000 0.500000 1.000000 10.50000 0.00469 0.00475 =
0.00449 -0.00041 0.00005 -0.00056
NA1 3 0.343386 0.275786 0.391339 11.00000 0.01282 0.01731 =
0.01064 -0.00157 0.00117 0.00001
O1 4 0.821546 0.436684 0.772978 11.00000 0.01031 0.00835 =
0.00585 0.00048 -0.00073 -0.00047
O2 4 0.846345 0.201361 1.016098 11.00000 0.00971 0.00651 =
0.00756 0.00050 -0.00009 -0.00159
O2A 4 0.640137 -0.080943 0.858591 11.00000 0.01289 0.00633 =
0.01277 -0.00096 0.00106 -0.00142
O1W 4 0.699201 0.612538 1.060570 11.00000 0.00666 0.00930 =
0.01065 0.00047 0.00285 0.00108
H1WA 2 0.688317 0.714792 1.014589 11.00000 -1.50000
PART -1
H1W 2 0.561911 0.548898 1.018955 10.50000 -1.50000
PART 0
O2W 4 0.277342 0.490250 0.615253 11.00000 0.01571 0.01929 =
0.01399 0.00103 0.00610 0.00263
H2WA 2 0.175612 0.574953 0.608253 11.00000 -1.50000
H2WB 2 0.276129 0.437391 0.701236 11.00000 -1.50000
O1A 4 0.601396 0.163429 0.611752 11.00000 0.04320 0.01159 =
0.01056 -0.00195 -0.01022 -0.00319
O3W 4 -0.078867 0.109917 0.336190 11.00000 0.01697 0.02670 =
0.01679 0.00550 0.00388 -0.00128
H3WA 2 -0.150270 0.105145 0.243914 11.00000 -1.50000
H3WB 2 -0.192877 0.059711 0.377259 11.00000 -1.50000
C1 1 0.716699 0.243496 0.740933 11.00000 0.01333 0.00827 =
0.00794 -0.00039 -0.00069 0.00112
C2 1 0.734587 0.106150 0.881499 11.00000 0.00702 0.00703 =
0.00826 -0.00012 0.00121 0.00106
HKLF 4
REM my_a.res in P-1
REM R1 = 0.0170 for 1975 Fo > 4sig(Fo) and 0.0172 for all 1984 data
REM 115 parameters refined using 6 restraints
END
WGHT 0.0000 0.2059
REM Highest difference peak 0.814, deepest hole -1.148, 1-sigma level 0.092
Q1 1 1.0387 0.4319 1.0647 11.00000 0.05 0.81
Q2 1 0.9954 0.3989 0.9319 11.00000 0.05 0.61
Q3 1 0.7224 0.1793 0.8160 11.00000 0.05 0.60
Q4 1 0.7968 0.5149 1.0239 11.00000 0.05 0.39
Q5 1 0.8786 0.3156 0.9939 11.00000 0.05 0.37
Q6 1 0.6656 0.0121 0.8957 11.00000 0.05 0.37
Q7 1 0.8851 0.4049 0.8645 11.00000 0.05 0.37
Q8 1 0.8445 0.3408 0.9937 11.00000 0.05 0.35
Q9 1 0.8170 0.5856 1.0554 11.00000 0.05 0.34
Q10 1 0.8287 0.4174 0.9399 11.00000 0.05 0.33
;
_shelx_res_checksum 97735
_shelx_hkl_file
;
-1 0 0 725.13 25.80
-1 0 0 712.53 25.80
1 0 0 725.93 25.80
-2 0 0 162.28 6.70
2 0 0 173.58 6.80
-3 0 0 2644.94 94.49
3 0 0 2643.44 94.49
-4 0 0 183.78 8.20
4 0 0 186.98 8.20
-5 0 0 165.28 6.60
-5 0 0 168.78 8.20
5 0 0 173.48 8.10
-6 0 0 622.14 24.60
-6 0 0 632.84 19.90
6 0 0 603.64 24.40
-7 0 0 362.76 16.40
-7 0 0 373.06 13.10
-8 1 0 275.37 11.20
-8 1 0 268.17 13.60
-7 1 0 301.57 14.10
-7 1 0 314.97 11.70
6 -1 0 396.46 16.70
-6 1 0 413.66 17.00
-6 1 0 408.26 13.90
5 -1 0 774.02 29.30
-5 1 0 773.42 29.50
-5 1 0 783.62 24.10
4 -1 0 472.65 17.70
-4 1 0 445.46 17.70
3 -1 0 983.60 34.00
-3 1 0 873.11 33.90
-3 1 0 938.61 34.00
2 -1 0 2145.39 75.79
-2 1 0 2020.70 74.99
-2 1 0 2147.09 76.09
1 -1 0 2511.85 93.79
1 -1 0 2720.53 93.79
-1 1 0 2544.15 93.59
-1 1 0 2650.73 93.69
0 -1 0 1631.24 60.59
0 -1 0 1758.72 60.79
0 1 0 1664.93 60.69
0 1 0 1681.33 60.69
-1 -1 0 752.92 26.30
-1 -1 0 711.13 26.30
1 1 0 724.23 26.30
-2 -1 0 414.06 15.70
2 1 0 421.26 15.80
-3 -1 0 501.25 19.00
3 1 0 504.75 19.10
-4 -1 0 2176.68 78.99
4 1 0 2199.78 78.99
-5 -1 0 108.99 4.80
-5 -1 0 112.99 6.30
5 1 0 116.89 6.40
-6 -1 0 790.02 29.00
-6 -1 0 697.83 22.90
6 1 0 721.23 28.70
-7 -1 0 539.25 18.20
-7 -1 0 583.24 23.50
-8 2 0 100.19 6.70
-8 2 0 115.89 7.90
-7 2 0 331.77 14.80
-7 2 0 316.57 12.30
-6 2 0 424.16 14.70
-6 2 0 427.46 17.70
5 -2 0 276.47 11.70
-5 2 0 282.77 10.00
-5 2 0 282.87 12.00
4 -2 0 491.75 18.70
-4 2 0 495.95 18.90
-4 2 0 483.65 15.50
3 -2 0 399.86 14.90
-3 2 0 358.46 14.80
-3 2 0 418.46 15.10
2 -2 0 1116.19 38.60
-2 2 0 1070.49 38.60
-2 2 0 1032.00 38.60
1 -2 0 226.88 8.20
-1 2 0 217.88 8.30
-1 2 0 215.18 8.30
0 -2 0 1080.29 37.80
0 2 0 985.80 37.70
0 2 0 1102.29 38.60
-1 -2 0 5014.20 170.68
1 2 0 4593.74 169.78
1 2 0 4574.34 170.38
-2 -2 0 604.14 22.40
-3 -2 0 515.45 19.40
3 2 0 496.25 19.40
-4 -2 0 1911.41 69.79
4 2 0 1935.21 69.89
-5 -2 0 725.03 28.00
5 2 0 726.23 28.10
-6 -2 0 32.40 4.10
6 2 0 32.70 3.90
-7 -2 0 197.38 10.70
-7 3 0 398.36 17.40
-7 3 0 409.46 14.80
-6 3 0 372.16 15.50
-6 3 0 358.26 13.00
5 -3 0 445.36 17.90
-5 3 0 463.45 15.30
-5 3 0 481.35 18.40
4 -3 0 448.06 16.40
-4 3 0 376.06 16.40
-4 3 0 438.56 16.70
-4 3 0 454.15 14.00
3 -3 0 481.45 17.60
-3 3 0 436.16 17.60
-3 3 0 497.25 17.90
2 -3 0 1397.66 48.80
-2 3 0 1394.16 48.90
-2 3 0 1404.76 48.90
-2 3 0 1242.68 48.80
1 -3 0 1511.75 55.49
-1 3 0 1599.94 54.89
-1 3 0 1488.75 54.89
0 -3 0 3547.34 121.79
0 3 0 3097.79 120.59
0 3 0 3454.45 121.29
-1 -3 0 1236.98 42.60
1 3 0 1187.48 42.70
1 3 0 1112.39 42.60
-2 -3 0 232.98 9.20
2 3 0 212.58 9.20
-3 -3 0 113.79 5.80
3 3 0 115.29 5.90
-4 -3 0 521.65 20.60
4 3 0 523.95 20.60
-5 -3 0 431.46 18.00
5 3 0 438.86 18.10
-6 -3 0 75.09 5.90
6 3 0 64.69 5.80
-7 -3 0 338.77 15.80
7 3 0 341.67 15.90
-7 4 0 377.86 14.50
-7 4 0 394.36 16.90
-6 4 0 737.13 27.60
-6 4 0 676.03 22.90
-5 4 0 18.70 2.70
-5 4 0 21.70 2.80
4 -4 0 197.78 8.50
-4 4 0 208.88 7.80
-4 4 0 214.08 9.00
3 -4 0 1183.38 40.90
-3 4 0 1160.48 33.70
-3 4 0 1022.50 41.00
-3 4 0 1154.08 41.20
2 -4 0 181.48 7.10
-2 4 0 166.58 7.20
-2 4 0 179.58 7.40
1 -4 0 2099.89 71.99
-1 4 0 1865.51 72.09
-1 4 0 2082.39 72.19
0 -4 0 696.63 24.50
0 4 0 691.13 24.70
0 4 0 610.94 24.50
-1 -4 0 21.20 2.00
1 4 0 12.10 1.90
-2 -4 0 538.15 20.30
2 4 0 530.55 20.50
-3 -4 0 275.17 11.70
3 4 0 278.97 11.80
-4 -4 0 691.83 26.80
4 4 0 696.73 27.00
-5 -4 0 896.21 35.10
5 4 0 935.51 35.40
-6 -4 0 251.37 12.30
6 4 0 256.57 12.60
-7 5 0 106.09 6.80
-7 5 0 118.39 7.40
-7 5 0 117.59 7.40
-6 5 0 52.99 4.70
-6 5 0 41.90 4.00
-6 5 0 45.70 4.30
-5 5 0 277.07 11.90
-5 5 0 270.07 11.90
-5 5 0 270.87 10.30
-4 5 0 259.67 9.50
-4 5 0 260.17 11.00
3 -5 0 661.53 25.00
-3 5 0 687.93 21.10
-3 5 0 690.13 25.50
2 -5 0 1209.68 42.50
-2 5 0 1211.68 35.00
-2 5 0 1211.08 42.90
-2 5 0 1074.59 42.70
1 -5 0 259.77 9.70
-1 5 0 243.88 10.00
-1 5 0 228.98 9.70
0 -5 0 1008.90 34.40
0 5 0 823.92 34.30
0 5 0 985.10 34.60
-1 -5 0 481.75 18.70
1 5 0 498.05 19.00
-2 -5 0 77.99 4.60
2 5 0 86.09 5.10
-3 -5 0 1522.95 56.39
3 5 0 1552.54 56.69
-4 -5 0 455.55 19.30
4 5 0 500.85 19.80
5 5 0 133.99 8.20
6 5 0 196.18 10.80
-6 6 0 112.19 7.00
-6 6 0 114.69 6.60
-5 6 0 625.74 20.30
-5 6 0 607.24 24.10
-4 6 0 450.45 15.00
-4 6 0 440.16 17.70
-3 6 0 133.29 5.80
-3 6 0 137.49 6.80
-2 6 0 942.41 34.30
-2 6 0 908.41 27.90
-1 6 0 487.05 18.90
0 -6 0 82.99 4.30
0 6 0 88.99 5.00
-1 -6 0 387.96 15.80
1 6 0 425.06 16.40
2 6 0 522.75 20.80
3 6 0 198.38 9.80
4 6 0 289.87 13.50
5 6 0 148.59 9.10
-6 7 0 195.78 9.20
-6 7 0 194.98 10.00
-5 7 0 8.50 2.70
-5 7 0 12.10 2.70
-4 7 0 245.08 10.90
-4 7 0 238.88 9.40
-3 7 0 492.75 15.90
-3 7 0 474.65 19.10
-2 7 0 131.59 6.80
-2 7 0 135.19 5.50
-1 7 0 521.15 20.50
0 7 0 332.37 14.00
1 7 0 255.97 11.50
2 7 0 378.96 16.10
3 7 0 175.28 9.40
4 7 0 393.86 17.60
-5 8 0 20.20 3.30
-5 8 0 26.40 3.40
-4 8 0 646.94 20.90
-4 8 0 630.24 25.00
-3 8 0 434.16 17.70
-3 8 0 431.16 14.60
-2 8 0 201.08 7.50
-2 8 0 203.48 9.60
-1 8 0 389.96 16.30
0 8 0 330.17 14.30
1 8 0 88.29 6.20
2 8 0 85.19 6.30
3 8 0 603.94 24.90
-3 9 0 477.55 16.10
-3 9 0 482.85 19.70
-2 9 0 70.69 5.40
-1 9 0 50.59 4.70
0 9 0 243.08 11.60
1 9 0 71.59 6.00
1 9 -1 122.09 7.40
0 9 -1 181.98 9.30
-1 9 -1 256.67 11.70
-2 9 -1 161.18 8.30
-3 9 -1 124.29 6.10
-3 9 -1 130.99 7.10
3 8 -1 291.97 13.80
2 8 -1 67.79 5.60
1 8 -1 72.69 5.40
0 8 -1 162.98 8.20
-1 8 -1 379.66 15.70
-2 8 -1 269.77 9.70
-2 8 -1 276.37 11.80
-3 8 -1 343.87 13.90
-3 8 -1 315.97 11.70
-4 8 -1 295.37 12.60
-4 8 -1 286.97 11.10
-5 8 -1 122.89 6.70
-5 8 -1 109.89 6.70
4 7 -1 14.90 3.30
3 7 -1 337.57 15.00
2 7 -1 262.57 11.90
1 7 -1 67.89 4.80
0 7 -1 851.11 32.00
-1 7 -1 546.35 20.90
-1 7 -1 537.05 16.90
-2 7 -1 665.03 20.70
-2 7 -1 665.33 25.30
-3 7 -1 289.97 10.50
-3 7 -1 295.67 12.20
-4 7 -1 19.00 2.70
-4 7 -1 15.50 2.60
-5 7 -1 247.38 10.10
-5 7 -1 245.58 11.10
-6 7 -1 273.77 12.20
-6 7 -1 244.68 10.80
5 6 -1 409.76 18.20
4 6 -1 87.59 6.40
3 6 -1 378.26 16.00
2 6 -1 1141.59 42.50
1 6 -1 111.49 5.90
0 6 -1 163.28 7.40
-1 6 -1 1884.01 55.09
-1 6 -1 1883.81 67.89
-2 6 -1 54.69 3.50
-2 6 -1 53.19 3.20
-3 6 -1 8.50 1.80
-3 6 -1 6.40 1.70
-4 6 -1 758.92 28.60
-4 6 -1 760.02 24.00
-5 6 -1 361.86 14.90
-5 6 -1 356.06 13.00
-6 6 -1 213.18 10.30
-6 6 -1 215.28 9.50
6 5 -1 123.99 8.30
5 5 -1 317.17 14.60
4 5 -1 675.23 25.60
-4 -5 1 618.44 25.10
3 5 -1 98.39 5.70
-3 -5 1 85.49 5.10
2 5 -1 401.56 15.80
-2 -5 1 388.06 15.40
1 5 -1 432.06 18.00
1 5 -1 501.25 18.40
-1 -5 1 495.85 18.00
0 5 -1 88.19 4.40
0 5 -1 100.39 4.80
0 -5 1 96.09 4.30
-1 5 -1 1180.68 41.80
1 -5 1 1124.39 41.30
-2 5 -1 827.92 32.10
-2 5 -1 929.61 32.30
-2 5 -1 891.61 26.60
-3 5 -1 260.87 8.90
-3 5 -1 243.98 10.20
-4 5 -1 732.13 23.10
-4 5 -1 742.23 27.70
-5 5 -1 568.14 21.80
-5 5 -1 568.34 21.80
-5 5 -1 540.85 18.40
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5 -2 -10 94.29 7.50
4 -2 -10 1077.49 41.60
3 -2 -10 204.38 10.60
2 -2 -10 211.78 10.60
1 -2 -10 628.94 25.10
0 -2 -10 52.29 4.90
-1 -2 -10 104.39 6.90
-2 -2 -10 87.19 6.50
5 -3 -10 97.29 7.60
4 -3 -10 412.76 18.40
3 -3 -10 249.48 12.30
2 -3 -10 48.20 5.00
1 -3 -10 387.06 16.80
0 -3 -10 331.07 15.00
-1 -3 -10 16.40 3.40
-2 -3 -10 667.43 27.30
4 -4 -10 106.09 7.70
3 -4 -10 587.34 24.50
2 -4 -10 235.88 11.90
1 -4 -10 112.39 7.50
0 -4 -10 476.65 20.50
-1 -4 -10 246.88 12.50
3 -5 -10 365.16 16.90
2 -5 -10 174.48 9.90
1 -5 -10 118.89 8.00
1 5 -11 319.97 12.60
3 4 -11 528.25 21.40
2 4 -11 125.69 6.70
1 4 -11 49.50 3.60
0 4 -11 316.47 12.40
-1 4 -11 209.28 8.30
4 3 -11 68.99 5.80
3 3 -11 408.66 17.30
2 3 -11 255.57 11.40
1 3 -11 209.98 9.40
0 3 -11 643.94 24.40
-1 3 -11 205.68 8.80
-2 3 -11 59.39 4.90
-2 3 -11 58.39 3.70
4 2 -11 73.29 6.30
3 2 -11 157.48 8.60
2 2 -11 781.22 30.00
1 2 -11 264.17 11.50
0 2 -11 9.10 2.10
-1 2 -11 290.67 12.20
-2 2 -11 130.69 6.70
5 1 -11 147.69 9.40
4 1 -11 158.38 9.10
3 1 -11 318.97 14.30
2 1 -11 617.44 24.50
1 1 -11 88.39 5.70
0 1 -11 106.99 6.10
-1 1 -11 360.66 15.10
-2 1 -11 343.07 14.60
5 0 -11 153.78 9.60
4 0 -11 515.85 21.80
3 0 -11 273.07 12.90
2 0 -11 172.08 9.00
1 0 -11 415.06 17.30
0 0 -11 75.39 5.20
-1 0 -11 202.68 9.90
-2 0 -11 523.35 21.30
5 -1 -11 16.40 3.90
4 -1 -11 176.08 10.00
3 -1 -11 486.05 20.60
2 -1 -11 90.09 6.40
1 -1 -11 212.58 10.50
0 -1 -11 385.56 16.50
-1 -1 -11 150.48 8.50
-2 -1 -11 204.18 10.40
4 -2 -11 267.77 13.50
3 -2 -11 442.56 19.10
2 -2 -11 435.76 18.70
1 -2 -11 74.99 6.10
0 -2 -11 351.06 15.60
-1 -2 -11 175.88 9.80
4 -3 -11 219.28 11.70
3 -3 -11 323.07 15.20
2 -3 -11 185.58 10.30
1 -3 -11 65.39 5.90
0 -3 -11 45.60 5.00
2 -4 -11 114.19 7.90
2 3 -12 241.18 11.10
1 3 -12 317.17 13.30
0 3 -12 80.29 4.70
3 2 -12 267.57 12.60
2 2 -12 553.14 22.30
1 2 -12 265.57 11.80
0 2 -12 82.79 5.20
-1 2 -12 147.09 7.40
3 1 -12 408.26 17.80
2 1 -12 87.09 6.20
1 1 -12 93.59 6.20
0 1 -12 165.88 8.40
-1 1 -12 104.09 6.40
3 0 -12 17.70 3.40
2 0 -12 300.47 13.80
1 0 -12 207.38 10.30
0 0 -12 135.29 7.70
-1 0 -12 539.05 22.10
3 -1 -12 102.89 7.40
2 -1 -12 142.49 8.50
1 -1 -12 422.76 18.10
0 -1 -12 181.88 9.70
2 -2 -12 77.29 6.60
1 -2 -12 285.07 13.50
0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 95863
_olex2_submission_special_instructions 'No special instructions were received'
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
Rh1 Rh 1.000000 0.500000 1.000000 0.00490(4) Uani 1 2 d S T P . .
Na1 Na 0.34339(11) 0.27579(10) 0.39134(7) 0.01407(12) Uani 1 1 d . . . . .
O1 O 0.82155(18) 0.43668(15) 0.77298(11) 0.00861(17) Uani 1 1 d . . . . .
O2 O 0.84634(17) 0.20136(15) 1.01610(11) 0.00840(17) Uani 1 1 d . . . . .
O2A O 0.64014(18) -0.08094(15) 0.85859(12) 0.01118(18) Uani 1 1 d . . . . .
O1W O 0.69920(17) 0.61254(16) 1.06057(12) 0.00876(17) Uani 1 1 d D . . . .
H1WA H 0.688(4) 0.715(3) 1.015(2) 0.013 Uiso 1 1 d DR . . . .
H1W H 0.562(5) 0.549(6) 1.019(5) 0.013 Uiso 0.5 1 d DR . . A -1
O2W O 0.2773(2) 0.49025(19) 0.61525(14) 0.0160(2) Uani 1 1 d D . . . .
H2WA H 0.176(4) 0.575(3) 0.608(3) 0.024 Uiso 1 1 d DR . . . .
H2WB H 0.276(5) 0.437(4) 0.701(2) 0.024 Uiso 1 1 d DR . . . .
O1A O 0.6014(3) 0.16343(19) 0.61175(14) 0.0244(3) Uani 1 1 d . . . . .
O3W O -0.0789(2) 0.1099(2) 0.33619(15) 0.0203(2) Uani 1 1 d D . . . .
H3WA H -0.150(5) 0.105(4) 0.244(2) 0.031 Uiso 1 1 d DR . . . .
H3WB H -0.193(4) 0.060(4) 0.377(3) 0.031 Uiso 1 1 d DR . . . .
C1 C 0.7167(3) 0.2435(2) 0.74093(16) 0.0103(2) Uani 1 1 d . . . . .
C2 C 0.7346(2) 0.1061(2) 0.88150(15) 0.0075(2) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Rh1 0.00469(6) 0.00475(6) 0.00449(7) -0.00041(4) 0.00005(4) -0.00056(4)
Na1 0.0128(3) 0.0173(3) 0.0106(3) -0.0016(2) 0.0012(2) 0.0000(2)
O1 0.0103(4) 0.0083(4) 0.0058(4) 0.0005(3) -0.0007(3) -0.0005(3)
O2 0.0097(4) 0.0065(4) 0.0076(4) 0.0005(3) -0.0001(3) -0.0016(3)
O2A 0.0129(4) 0.0063(4) 0.0128(4) -0.0010(3) 0.0011(3) -0.0014(3)
O1W 0.0067(4) 0.0093(4) 0.0106(4) 0.0005(3) 0.0028(3) 0.0011(3)
O2W 0.0157(5) 0.0193(5) 0.0140(5) 0.0010(4) 0.0061(4) 0.0026(4)
O1A 0.0432(7) 0.0116(5) 0.0106(5) -0.0019(4) -0.0102(5) -0.0032(5)
O3W 0.0170(5) 0.0267(6) 0.0168(5) 0.0055(5) 0.0039(4) -0.0013(4)
C1 0.0133(5) 0.0083(5) 0.0079(5) -0.0004(4) -0.0007(4) 0.0011(4)
C2 0.0070(5) 0.0070(5) 0.0083(5) -0.0001(4) 0.0012(4) 0.0011(4)
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'
Na Na 0.0362 0.0249 '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'
Rh Rh -1.1178 0.9187 '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 Rh1 O1 180.0 . 2_767 ?
O1 Rh1 O1W 89.72(5) . . ?
O1 Rh1 O1W 90.28(5) 2_767 . ?
O1 Rh1 O1W 89.72(5) 2_767 2_767 ?
O1 Rh1 O1W 90.28(5) . 2_767 ?
O2 Rh1 O1 97.36(5) 2_767 . ?
O2 Rh1 O1 82.64(5) . . ?
O2 Rh1 O1 82.64(5) 2_767 2_767 ?
O2 Rh1 O1 97.36(5) . 2_767 ?
O2 Rh1 O2 180.0 2_767 . ?
O2 Rh1 O1W 88.78(5) . 2_767 ?
O2 Rh1 O1W 91.22(5) . . ?
O2 Rh1 O1W 91.22(5) 2_767 2_767 ?
O2 Rh1 O1W 88.78(5) 2_767 . ?
O1W Rh1 O1W 180.0 2_767 . ?
O1 Na1 Na1 78.44(4) 2_666 2_666 ?
O1 Na1 O1A 145.39(4) 2_666 2_656 ?
O2A Na1 Na1 136.52(5) 2_656 2_666 ?
O2A Na1 O1 87.27(4) 2_656 2_666 ?
O2A Na1 O1A 61.11(4) 2_656 2_656 ?
O2W Na1 Na1 45.35(4) . 2_666 ?
O2W Na1 Na1 44.67(4) 2_666 2_666 ?
O2W Na1 O1 78.69(5) 2_666 2_666 ?
O2W Na1 O1 85.03(4) . 2_666 ?
O2W Na1 O2A 92.47(5) 2_666 2_656 ?
O2W Na1 O2A 171.28(5) . 2_656 ?
O2W Na1 O2W 90.02(5) . 2_666 ?
O2W Na1 O1A 125.11(5) . 2_656 ?
O2W Na1 O1A 76.15(5) . . ?
O2W Na1 O1A 113.96(5) 2_666 2_656 ?
O1A Na1 Na1 133.89(4) 2_656 2_666 ?
O1A Na1 Na1 74.00(4) . 2_666 ?
O1A Na1 O1 152.43(5) . 2_666 ?
O1A Na1 O2A 112.48(5) . 2_656 ?
O1A Na1 O2W 81.32(5) . 2_666 ?
O1A Na1 O1A 61.20(5) . 2_656 ?
O3W Na1 Na1 134.80(5) . 2_666 ?
O3W Na1 O1 83.95(5) . 2_666 ?
O3W Na1 O2A 82.91(5) . 2_656 ?
O3W Na1 O2W 162.24(5) . 2_666 ?
O3W Na1 O2W 92.21(6) . . ?
O3W Na1 O1A 116.31(6) . . ?
O3W Na1 O1A 78.79(5) . 2_656 ?
Rh1 O1 Na1 122.51(5) . 2_666 ?
C1 O1 Rh1 112.54(9) . . ?
C1 O1 Na1 119.86(8) . 2_666 ?
C2 O2 Rh1 112.78(9) . . ?
C2 O2A Na1 118.35(9) . 2_656 ?
Rh1 O1W H1WA 105.2(16) . . ?
Rh1 O1W H1W 117(3) . . ?
H1WA O1W H1W 95(4) . . ?
Na1 O2W Na1 89.98(5) . 2_666 ?
Na1 O2W H2WA 122.8(17) . . ?
Na1 O2W H2WA 100.8(17) 2_666 . ?
Na1 O2W H2WB 118.5(17) . . ?
Na1 O2W H2WB 113.4(18) 2_666 . ?
H2WA O2W H2WB 108(2) . . ?
Na1 O1A Na1 118.80(5) . 2_656 ?
C1 O1A Na1 104.44(10) . 2_656 ?
C1 O1A Na1 136.60(10) . . ?
Na1 O3W H3WA 116.3(19) . . ?
Na1 O3W H3WB 143.4(19) . . ?
H3WA O3W H3WB 100(3) . . ?
O1 C1 C2 115.81(11) . . ?
O1A C1 O1 125.71(13) . . ?
O1A C1 C2 118.46(13) . . ?
O2 C2 C1 115.75(11) . . ?
O2A C2 O2 125.11(13) . . ?
O2A C2 C1 119.13(12) . . ?
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
Rh1 O1 2.0221(11) 2_767 ?
Rh1 O1 2.0221(11) . ?
Rh1 O2 2.0150(11) 2_767 ?
Rh1 O2 2.0151(11) . ?
Rh1 O1W 2.0377(10) 2_767 ?
Rh1 O1W 2.0378(10) . ?
Na1 Na1 3.4033(18) 2_666 ?
Na1 O1 2.5879(13) 2_666 ?
Na1 O2A 2.4277(14) 2_656 ?
Na1 O2W 2.4211(15) 2_666 ?
Na1 O2W 2.3928(15) . ?
Na1 O1A 2.8864(15) 2_656 ?
Na1 O1A 2.4012(15) . ?
Na1 O3W 2.3907(16) . ?
O1 C1 1.2868(17) . ?
O2 C2 1.2854(16) . ?
O2A C2 1.2324(16) . ?
O1W H1WA 0.797(15) . ?
O1W H1W 0.823(19) . ?
O2W H2WA 0.837(16) . ?
O2W H2WB 0.836(16) . ?
O1A C1 1.2239(18) . ?
O3W H3WA 0.823(17) . ?
O3W H3WB 0.813(17) . ?
C1 C2 1.5467(19) . ?
_cod_database_fobs_code 2108901