#------------------------------------------------------------------------------
#$Date: 2020-02-04 22:08:36 +0200 (Tue, 04 Feb 2020) $
#$Revision: 247611 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/56/7125658.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_7125658
loop_
_publ_author_name
'Li, Jing-Yu'
'Tian, Yu-Chen'
'Feng, Li-Na'
'Zhou, Zi-Qin'
'Wang, Lin-Lin'
'Yang, Jian-Hui'
'Liu, Bin'
_publ_section_title
;
Enhancing magnetic hardness by sonication assisted synthesis of
heterometallic carbonato spin-glass
Na[Ni(H2O)4Ru2(CO3)4]·3H2O.
;
_journal_issue 9
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first 1369
_journal_page_last 1372
_journal_paper_doi 10.1039/c9cc07876b
_journal_volume 56
_journal_year 2020
_chemical_formula_moiety 'C4 H8 Na Ni O16 Ru2, 3(H2O)'
_chemical_formula_sum 'C4 H14 Na Ni O19 Ru2'
_chemical_formula_weight 649.99
_space_group_crystal_system orthorhombic
_space_group_IT_number 56
_space_group_name_Hall '-P 2ab 2ac'
_space_group_name_H-M_alt 'P c c n'
_atom_sites_solution_hydrogens difmap
_audit_creation_method SHELXL-2018/3
_audit_update_record
;
2019-03-07 deposited with the CCDC. 2019-12-16 downloaded from the CCDC.
;
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 18.251(3)
_cell_length_b 9.2828(16)
_cell_length_c 10.1645(17)
_cell_measurement_reflns_used 386
_cell_measurement_temperature 296(2)
_cell_measurement_theta_max 23.807
_cell_measurement_theta_min 2.231
_cell_volume 1722.1(5)
_computing_cell_refinement 'Bruker SAINT'
_computing_data_collection 'Bruker APEX2'
_computing_data_reduction 'Bruker SAINT'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature 296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0577
_diffrn_reflns_av_unetI/netI 0.0436
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max 22
_diffrn_reflns_limit_h_min -21
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -6
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_number 8614
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 26.119
_diffrn_reflns_theta_min 2.232
_exptl_absorpt_coefficient_mu 2.936
_exptl_absorpt_correction_T_max 0.891
_exptl_absorpt_correction_T_min 0.710
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details sadabs
_exptl_crystal_colour brown
_exptl_crystal_density_diffrn 2.507
_exptl_crystal_description block
_exptl_crystal_F_000 1268
_exptl_crystal_size_max 0.120
_exptl_crystal_size_mid 0.100
_exptl_crystal_size_min 0.040
_refine_diff_density_max 1.467
_refine_diff_density_min -0.626
_refine_diff_density_rms 0.163
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.059
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 150
_refine_ls_number_reflns 1714
_refine_ls_number_restraints 24
_refine_ls_restrained_S_all 1.062
_refine_ls_R_factor_all 0.0530
_refine_ls_R_factor_gt 0.0368
_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^)+(0.0631P)^2^+0.6477P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0991
_refine_ls_wR_factor_ref 0.1080
_reflns_Friedel_coverage 0.000
_reflns_number_gt 1347
_reflns_number_total 1714
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file c9cc07876b2.cif
_cod_data_source_block xb0484
_cod_depositor_comments 'Adding full bibliography for 7125658.cif.'
_cod_database_code 7125658
_shelx_shelxl_version_number 2018/3
_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_min 0.720
_shelx_estimated_absorpt_t_max 0.892
_shelx_res_file
;
TITL xb0484 in Pccn
xb0484.res
created by SHELXL-2018/3 at 15:08:02 on 05-Mar-2019
CELL 0.71073 18.2511 9.2828 10.1645 90.000 90.000 90.000
ZERR 1.00 0.0033 0.0016 0.0017 0.000 0.000 0.000
LATT 1
SYMM 0.5-X, 0.5-Y, Z
SYMM -X, 0.5+Y, 0.5-Z
SYMM 0.5+X, -Y, 0.5-Z
SFAC C H O Ni Ru Na
UNIT 16 56 76 4 8 4
L.S. 15
ACTA
BOND $H
FMAP 2
PLAN 5
SIZE 0.04 0.10 0.12
htab
EQIV $9 x, -y+1/2, z+1/2
HTAB O7 O3_$9
HTAB O7 O2
HTAB O8 O2
HTAB O8 O1_$9
FREE O9' Na1
FREE O9 O9'
FREE O10 O10'
FREE O9 O10'
FREE O9' O10'
FREE O9' O10
FREE O9 O10
ISOR 0.02 O9 O9' O10 O10'
TEMP 23.000
WGHT 0.063100 0.647700
FVAR 0.07717
MOLE 1
O1 3 0.620803 0.006654 0.430469 11.00000 0.02014 0.02591 =
0.01435 -0.00237 -0.00029 -0.00435
O5 3 0.539224 -0.233676 0.521531 11.00000 0.04358 0.01047 =
0.01713 0.00212 0.00428 0.00171
O6 3 0.551617 -0.335757 0.715684 11.00000 0.04860 0.02184 =
0.01910 0.01255 0.01064 0.01185
RU1 5 0.483714 0.061461 0.591461 11.00000 0.01907 0.01216 =
0.00990 -0.00078 0.00065 -0.00179
NI1 4 0.750000 0.250000 0.685315 10.50000 0.02546 0.03350 =
0.01344 0.00000 0.00000 -0.00943
O4 3 0.504954 -0.114633 0.703930 11.00000 0.02795 0.01794 =
0.01473 0.00434 0.00406 0.00635
O3 3 0.703829 0.126625 0.542113 11.00000 0.02407 0.03432 =
0.01839 -0.00741 0.00288 -0.00607
O2 3 0.589056 0.126064 0.613867 11.00000 0.02131 0.02803 =
0.01580 -0.00707 0.00228 -0.00956
O7 3 0.709760 0.116933 0.826887 11.00000 0.05340 0.09024 =
0.02278 0.01137 -0.00922 -0.03977
AFIX 3
H7B 2 0.699910 0.164804 0.896217 11.00000 -1.50000
H7C 2 0.671270 0.077783 0.797867 11.00000 -1.50000
AFIX 0
C2 1 0.531069 -0.229115 0.649347 11.00000 0.02449 0.02271 =
0.01550 0.00296 0.00378 0.00056
C1 1 0.638577 0.086554 0.529342 11.00000 0.02389 0.01849 =
0.01293 -0.00275 -0.00042 -0.00046
O8 3 0.657755 0.385795 0.681939 11.00000 0.03558 0.04514 =
0.03809 -0.01584 0.00669 -0.00077
AFIX 3
H8B 2 0.621586 0.334775 0.659807 11.00000 -1.50000
H8C 2 0.650226 0.421785 0.758159 11.00000 -1.50000
AFIX 0
NA1 6 0.579261 -0.520180 0.434197 10.50000 0.06204 0.04794 =
0.04578 -0.01234 -0.00569 0.01507
O9 3 0.728163 0.714144 0.585528 10.50000 0.20824 0.19938 =
0.26729 -0.01782 -0.00267 0.06392
O9' 3 0.707091 0.682213 0.495265 10.50000 0.08382 0.10117 =
0.23045 -0.03550 -0.01908 0.00585
O10 3 0.718196 0.804953 0.761525 10.25000 0.20202 0.19339 =
0.21580 -0.00636 -0.02658 -0.02808
O10' 3 0.709523 0.652472 0.748094 10.25000 0.09356 0.08270 =
0.11108 -0.04475 -0.04861 0.05961
HKLF 4
REM xb0484 in Pccn
REM wR2 = 0.1080, GooF = S = 1.059, Restrained GooF = 1.062 for all data
REM R1 = 0.0368 for 1347 Fo > 4sig(Fo) and 0.0530 for all 1714 data
REM 150 parameters refined using 24 restraints
END
WGHT 0.0629 0.5621
REM Instructions for potential hydrogen bonds
HTAB O7 O3_$9
HTAB O7 O2
HTAB O8 O2
HTAB O8 O1_$9
REM Highest difference peak 1.467, deepest hole -0.626, 1-sigma level 0.163
Q1 1 0.6205 -0.4215 0.5744 11.00000 0.05 1.47
Q2 1 0.7178 0.7181 0.6726 11.00000 0.05 0.87
Q3 1 0.7500 0.7500 0.5490 10.50000 0.05 0.83
Q4 1 0.5910 -0.5541 0.3990 11.00000 0.05 0.80
Q5 1 0.5935 -0.4311 0.4600 11.00000 0.05 0.71
;
_shelx_res_checksum 96429
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, 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
O1 O 0.6208(2) 0.0067(5) 0.4305(4) 0.0201(9) Uani 1 1 d . . .
O5 O 0.5392(2) -0.2337(4) 0.5215(4) 0.0237(10) Uani 1 1 d . . .
O6 O 0.5516(3) -0.3358(5) 0.7157(4) 0.0298(11) Uani 1 1 d . . .
Ru1 Ru 0.48371(3) 0.06146(5) 0.59146(4) 0.01371(18) Uani 1 1 d . . .
Ni1 Ni 0.750000 0.250000 0.68531(10) 0.0241(3) Uani 1 2 d S T P
O4 O 0.5050(2) -0.1146(5) 0.7039(4) 0.0202(9) Uani 1 1 d . . .
O3 O 0.7038(2) 0.1266(5) 0.5421(4) 0.0256(10) Uani 1 1 d . . .
O2 O 0.5891(2) 0.1261(5) 0.6139(4) 0.0217(9) Uani 1 1 d . . .
O7 O 0.7098(3) 0.1169(7) 0.8269(5) 0.0555(17) Uani 1 1 d . . .
H7B H 0.699910 0.164804 0.896217 0.083 Uiso 1 1 d R U .
H7C H 0.671270 0.077783 0.797867 0.083 Uiso 1 1 d R U .
C2 C 0.5311(3) -0.2291(7) 0.6493(6) 0.0209(14) Uani 1 1 d . . .
C1 C 0.6386(3) 0.0866(6) 0.5293(5) 0.0184(13) Uani 1 1 d . . .
O8 O 0.6578(3) 0.3858(5) 0.6819(5) 0.0396(13) Uani 1 1 d . . .
H8B H 0.621586 0.334775 0.659807 0.059 Uiso 1 1 d R U .
H8C H 0.650226 0.421785 0.758159 0.059 Uiso 1 1 d R U .
Na1 Na 0.5793(4) -0.5202(7) 0.4342(6) 0.0519(17) Uani 0.5 1 d . . P
O9 O 0.728(3) 0.714(6) 0.586(4) 0.22(2) Uani 0.5 1 d . U P
O9' O 0.7071(12) 0.682(3) 0.495(3) 0.138(9) Uani 0.5 1 d . U P
O10 O 0.718(4) 0.805(7) 0.762(6) 0.20(3) Uani 0.25 1 d . U P
O10' O 0.7095(19) 0.652(4) 0.748(4) 0.096(11) Uani 0.25 1 d . U P
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
O1 0.020(2) 0.026(2) 0.014(2) -0.0024(18) -0.0003(16) -0.0043(19)
O5 0.044(3) 0.010(2) 0.017(2) 0.0021(16) 0.0043(19) 0.0017(19)
O6 0.049(3) 0.022(3) 0.019(2) 0.0125(18) 0.011(2) 0.012(2)
Ru1 0.0191(3) 0.0122(3) 0.0099(3) -0.00078(17) 0.00065(17) -0.00179(18)
Ni1 0.0255(6) 0.0335(7) 0.0134(5) 0.000 0.000 -0.0094(5)
O4 0.028(2) 0.018(2) 0.015(2) 0.0043(17) 0.0041(16) 0.0064(18)
O3 0.024(2) 0.034(3) 0.018(2) -0.0074(19) 0.0029(18) -0.006(2)
O2 0.021(2) 0.028(3) 0.016(2) -0.0071(17) 0.0023(17) -0.0096(19)
O7 0.053(4) 0.090(5) 0.023(3) 0.011(3) -0.009(2) -0.040(3)
C2 0.024(3) 0.023(4) 0.016(3) 0.003(3) 0.004(2) 0.001(3)
C1 0.024(3) 0.018(3) 0.013(3) -0.003(2) 0.000(2) 0.000(2)
O8 0.036(3) 0.045(3) 0.038(3) -0.016(2) 0.007(2) -0.001(2)
Na1 0.062(5) 0.048(4) 0.046(4) -0.012(3) -0.006(3) 0.015(3)
O9 0.21(3) 0.20(3) 0.27(3) -0.018(19) -0.003(19) 0.064(19)
O9' 0.084(14) 0.101(15) 0.23(3) -0.036(18) -0.019(16) 0.006(10)
O10 0.20(3) 0.19(3) 0.22(3) -0.01(2) -0.027(19) -0.028(19)
O10' 0.09(2) 0.08(2) 0.11(2) -0.045(17) -0.049(18) 0.060(16)
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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 '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'
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
C1 O1 Ru1 120.2(4) . 5_656
C2 O5 Ru1 121.2(4) . 5_656
C2 O5 Na1 111.3(4) . .
Ru1 O5 Na1 127.4(2) 5_656 .
C2 O6 Ru1 135.2(4) . 3_646
O5 Ru1 O1 89.38(18) 5_656 5_656
O5 Ru1 O2 91.51(18) 5_656 .
O1 Ru1 O2 178.98(17) 5_656 .
O5 Ru1 O4 178.77(18) 5_656 .
O1 Ru1 O4 89.45(17) 5_656 .
O2 Ru1 O4 89.65(17) . .
O5 Ru1 Ru1 89.21(12) 5_656 5_656
O1 Ru1 Ru1 89.98(11) 5_656 5_656
O2 Ru1 Ru1 89.56(11) . 5_656
O4 Ru1 Ru1 90.37(12) . 5_656
O5 Ru1 O6 95.72(16) 5_656 3_656
O1 Ru1 O6 87.63(16) 5_656 3_656
O2 Ru1 O6 92.75(16) . 3_656
O4 Ru1 O6 84.64(16) . 3_656
Ru1 Ru1 O6 174.49(11) 5_656 3_656
O7 Ni1 O7 89.9(3) 2_655 .
O7 Ni1 O3 176.0(2) 2_655 .
O7 Ni1 O3 90.85(19) . .
O7 Ni1 O3 90.85(19) 2_655 2_655
O7 Ni1 O3 176.0(2) . 2_655
O3 Ni1 O3 88.7(2) . 2_655
O7 Ni1 O8 95.0(2) 2_655 2_655
O7 Ni1 O8 86.4(2) . 2_655
O3 Ni1 O8 89.00(19) . 2_655
O3 Ni1 O8 89.67(18) 2_655 2_655
O7 Ni1 O8 86.4(2) 2_655 .
O7 Ni1 O8 95.0(2) . .
O3 Ni1 O8 89.67(18) . .
O3 Ni1 O8 89.00(19) 2_655 .
O8 Ni1 O8 178.1(3) 2_655 .
C2 O4 Ru1 119.4(4) . .
C2 O4 Na1 121.0(4) . 7_556
Ru1 O4 Na1 101.0(2) . 7_556
C1 O3 Ni1 129.4(4) . .
C1 O2 Ru1 120.1(4) . .
Ni1 O7 Na1 141.8(3) . 7_556
Ni1 O7 H7B 110.2 . .
Na1 O7 H7B 70.2 7_556 .
Ni1 O7 H7C 108.3 . .
Na1 O7 H7C 44.1 7_556 .
H7B O7 H7C 109.7 . .
O6 C2 O4 121.9(5) . .
O6 C2 O5 118.3(5) . .
O4 C2 O5 119.7(5) . .
O3 C1 O1 119.3(5) . .
O3 C1 O2 120.5(5) . .
O1 C1 O2 120.1(5) . .
Ni1 O8 H8B 107.1 . .
Ni1 O8 H8C 110.4 . .
H8B O8 H8C 109.6 . .
O7 Na1 O5 129.4(3) 7 .
O7 Na1 O4 102.6(2) 7 7
O5 Na1 O4 75.0(2) . 7
O7 Na1 Na1 167.8(4) 7 5_646
O5 Na1 Na1 62.5(2) . 5_646
O4 Na1 Na1 82.4(3) 7 5_646
O9 O9 O9' 31.1(14) 2_665 2_665
O10' O10 O10 58(4) 2_665 2_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 C1 1.290(7) .
O1 Ru1 2.022(4) 5_656
O5 C2 1.308(7) .
O5 Ru1 2.012(4) 5_656
O5 Na1 2.897(8) .
O6 C2 1.255(7) .
O6 Ru1 2.273(4) 3_646
Ru1 O2 2.027(4) .
Ru1 O4 2.032(4) .
Ru1 Ru1 2.2611(9) 5_656
Ni1 O7 2.034(5) 2_655
Ni1 O7 2.034(5) .
Ni1 O3 2.035(4) .
Ni1 O3 2.035(4) 2_655
Ni1 O8 2.103(5) 2_655
Ni1 O8 2.103(5) .
O4 C2 1.290(7) .
O4 Na1 2.981(8) 7_556
O3 C1 1.254(7) .
O2 C1 1.300(7) .
O7 Na1 2.769(8) 7_556
O7 H7B 0.8523 .
O7 H7C 0.8441 .
O8 H8B 0.8430 .
O8 H8C 0.8548 .
Na1 Na1 3.209(14) 5_646
O9 O9 1.04(10) 2_665
O9 O9' 1.78(5) 2_665
O10 O10' 1.38(7) 2_665
O10 O10 1.55(12) 2_665
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O7 H7B O3 0.85 2.44 3.235(7) 155.5 7_566 yes
O7 H7C O2 0.84 2.44 3.090(6) 134.5 . yes
O8 H8B O2 0.84 2.08 2.804(6) 143.8 . yes
O8 H8C O1 0.85 1.95 2.799(6) 172.8 7_566 yes