#------------------------------------------------------------------------------
#$Date: 2019-11-08 00:07:59 +0100 (vie 08 de nov de 2019) $
#$Revision: 224422 $
#$URL: svn://www.crystallography.net/cod/cif/7/04/99/7049931.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_7049931
loop_
_publ_author_name
'Fan, Xiao-Meng'
'Li, Jing-Yu'
'Wang, Lin-Lin'
'Zhou, Zi-Qin'
'Tian, Yu-Chen'
'Yang, Jian-Hui'
'Liu, Bin'
_publ_section_title
;
 Alkali counterions tune diruthenium(iii,iii)-based ferrimagnetic chain
 structured antiferromagnets exhibiting step-like hysteresis loops.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8039
_journal_page_last               8043
_journal_paper_doi               10.1039/c9dt01295h
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'Cu H14 O22 P4 Ru2, 2(H2 O), 2(K)'
_chemical_formula_sum            'Cu H18 K2 O24 P4 Ru2'
_chemical_formula_weight         869.90
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-04-29 deposited with the CCDC.    2019-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                87.824(2)
_cell_angle_beta                 76.102(2)
_cell_angle_gamma                64.533(2)
_cell_formula_units_Z            1
_cell_length_a                   7.7337(12)
_cell_length_b                   8.4478(13)
_cell_length_c                   9.1576(14)
_cell_measurement_reflns_used    2500
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.15
_cell_measurement_theta_min      2.68
_cell_volume                     522.89(14)
_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 0.988
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            2956
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.157
_diffrn_reflns_theta_min         2.297
_exptl_absorpt_coefficient_mu    3.250
_exptl_absorpt_correction_T_max  0.783
_exptl_absorpt_correction_T_min  0.732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.763
_exptl_crystal_description       block
_exptl_crystal_F_000             425
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.220
_refine_diff_density_max         0.966
_refine_diff_density_min         -1.111
_refine_diff_density_rms         0.144
_refine_ls_extinction_coef       0.024(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         2153
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0310
_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)+(0.0371P)²+0.8101P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0852
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2079
_reflns_number_total             2153
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt01295h2.cif
_cod_data_source_block           xb1008_0m
_cod_depositor_comments
'Adding full bibliography for 7049930--7049933.cif.'
_cod_database_code               7049931
_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   0.442
_shelx_estimated_absorpt_t_max   0.535
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
Ru1 Ru 0.39793(4) 0.07444(3) 0.91921(3) 0.01160(14) Uani 1 1 d . . .
Cu1 Cu 1.000000 0.000000 0.500000 0.01682(18) Uani 1 2 d S . P
K1 K 1.17253(15) -0.31375(15) 0.83626(13) 0.0415(3) Uani 1 1 d . . .
P1 P 0.78591(13) 0.11767(12) 0.84467(9) 0.0136(2) Uani 1 1 d . . .
P2 P 0.30558(14) 0.30638(12) 1.20566(10) 0.0167(2) Uani 1 1 d . . .
O1 O 0.7901(4) 0.0261(3) 0.9963(3) 0.0165(5) Uani 1 1 d . . .
O2 O 0.5724(4) 0.1837(3) 0.8225(3) 0.0173(5) Uani 1 1 d . . .
O3 O 0.8283(4) 0.2757(3) 0.8564(3) 0.0196(5) Uani 1 1 d . . .
O4 O 0.9358(4) -0.0173(3) 0.7179(3) 0.0198(5) Uani 1 1 d . . .
O5 O 0.2346(4) 0.2822(3) 1.0666(3) 0.0200(5) Uani 1 1 d . . .
O6 O 0.4522(4) 0.1238(3) 1.2407(3) 0.0197(5) Uani 1 1 d . . .
O7 O 0.1345(5) 0.4000(4) 1.3359(3) 0.0320(7) Uani 1 1 d . . .
O8 O 0.4333(4) 0.4108(4) 1.1600(3) 0.0243(6) Uani 1 1 d D . .
O9 O 0.2102(4) 0.2042(4) 0.7553(3) 0.0243(6) Uani 1 1 d . . .
H9B H 0.090947 0.224250 0.795721 0.036 Uiso 1 1 d R U .
H9C H 0.216377 0.300580 0.733361 0.036 Uiso 1 1 d R U .
O10 O 1.0814(5) -0.2662(4) 0.4823(3) 0.0324(7) Uani 1 1 d . . .
H10A H 0.981928 -0.283395 0.478673 0.049 Uiso 1 1 d R U .
H10B H 1.172418 -0.312495 0.402273 0.049 Uiso 1 1 d R U .
O11 O 1.3193(5) -0.0555(5) 0.5025(3) 0.0397(8) Uani 1 1 d . . .
H11A H 1.326112 0.041493 0.509995 0.060 Uiso 1 1 d R U .
H11B H 1.349842 -0.114037 0.577425 0.060 Uiso 1 1 d R U .
O12 O 1.3560(6) -0.5826(5) 0.6002(5) 0.0533(10) Uani 1 1 d . . .
H12A H 1.443606 -0.672477 0.627456 0.080 Uiso 1 1 d R U .
H12B H 1.409926 -0.546647 0.522466 0.080 Uiso 1 1 d R U .
H1 H 0.363(8) 0.518(3) 1.152(7) 0.056(18) Uiso 1 1 d D . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cu Cu 0.3201 1.2651 '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'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
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
O2 Ru1 O1 175.21(9) . 2_657
O2 Ru1 O5 90.99(11) . .
O1 Ru1 O5 89.18(11) 2_657 .
O2 Ru1 O6 88.73(11) . 2_657
O1 Ru1 O6 90.70(11) 2_657 2_657
O5 Ru1 O6 175.19(10) . 2_657
O2 Ru1 O9 87.76(10) . .
O1 Ru1 O9 87.45(10) 2_657 .
O5 Ru1 O9 90.24(11) . .
O6 Ru1 O9 84.94(11) 2_657 .
O2 Ru1 Ru1 92.55(7) . 2_657
O1 Ru1 Ru1 92.23(7) 2_657 2_657
O5 Ru1 Ru1 92.85(8) . 2_657
O6 Ru1 Ru1 91.96(8) 2_657 2_657
O9 Ru1 Ru1 176.88(8) . 2_657
O2 Ru1 K1 128.37(8) . 2_657
O1 Ru1 K1 49.96(8) 2_657 2_657
O5 Ru1 K1 43.48(8) . 2_657
O6 Ru1 K1 134.36(8) 2_657 2_657
O9 Ru1 K1 72.87(7) . 2_657
Ru1 Ru1 K1 109.23(2) 2_657 2_657
O4 Cu1 O4 180.0 . 2_756
O4 Cu1 O10 85.96(11) . .
O4 Cu1 O10 94.04(11) 2_756 .
O4 Cu1 O10 94.04(11) . 2_756
O4 Cu1 O10 85.96(11) 2_756 2_756
O10 Cu1 O10 180.0 . 2_756
O4 Cu1 O11 90.26(11) . .
O4 Cu1 O11 89.74(11) 2_756 .
O10 Cu1 O11 90.01(13) . .
O10 Cu1 O11 89.99(13) 2_756 .
O4 Cu1 O11 89.74(11) . 2_756
O4 Cu1 O11 90.26(11) 2_756 2_756
O10 Cu1 O11 89.99(13) . 2_756
O10 Cu1 O11 90.01(13) 2_756 2_756
O11 Cu1 O11 180.0 . 2_756
O4 K1 O8 125.72(9) . 2_757
O4 K1 O12 106.09(10) . .
O8 K1 O12 81.80(11) 2_757 .
O4 K1 O3 116.31(8) . 2_757
O8 K1 O3 73.90(8) 2_757 2_757
O12 K1 O3 137.60(11) . 2_757
O4 K1 O5 73.10(8) . 2_657
O8 K1 O5 158.88(9) 2_757 2_657
O12 K1 O5 103.30(11) . 2_657
O3 K1 O5 89.44(8) 2_757 2_657
O4 K1 O1 79.18(8) . 2_757
O8 K1 O1 68.87(8) 2_757 2_757
O12 K1 O1 145.89(11) . 2_757
O3 K1 O1 50.13(7) 2_757 2_757
O5 K1 O1 110.35(8) 2_657 2_757
O4 K1 O1 49.20(7) . .
O8 K1 O1 128.23(8) 2_757 .
O12 K1 O1 147.66(10) . .
O3 K1 O1 70.77(7) 2_757 .
O5 K1 O1 53.88(7) 2_657 .
O1 K1 O1 59.50(8) 2_757 .
O4 K1 P1 100.11(6) . 2_757
O8 K1 P1 67.41(6) 2_757 2_757
O12 K1 P1 147.62(10) . 2_757
O3 K1 P1 24.31(5) 2_757 2_757
O5 K1 P1 102.26(6) 2_657 2_757
O1 K1 P1 25.98(5) 2_757 2_757
O1 K1 P1 64.71(5) . 2_757
O4 K1 P2 65.03(6) . 2_657
O8 K1 P2 165.10(7) 2_757 2_657
O12 K1 P2 85.12(9) . 2_657
O3 K1 P2 112.10(6) 2_757 2_657
O5 K1 P2 22.70(5) 2_657 2_657
O1 K1 P2 125.71(6) 2_757 2_657
O1 K1 P2 66.21(5) . 2_657
P1 K1 P2 123.73(4) 2_757 2_657
O4 K1 Ru1 65.39(6) . 2_657
O8 K1 Ru1 144.63(7) 2_757 2_657
O12 K1 Ru1 130.56(9) . 2_657
O3 K1 Ru1 71.72(6) 2_757 2_657
O5 K1 Ru1 27.58(5) 2_657 2_657
O1 K1 Ru1 82.78(5) 2_757 2_657
O1 K1 Ru1 28.47(5) . 2_657
P1 K1 Ru1 77.80(3) 2_757 2_657
P2 K1 Ru1 46.15(2) 2_657 2_657
O3 P1 O4 112.60(15) . .
O3 P1 O2 108.56(14) . .
O4 P1 O2 110.71(15) . .
O3 P1 O1 109.35(15) . .
O4 P1 O1 108.20(14) . .
O2 P1 O1 107.29(14) . .
O3 P1 K1 50.43(11) . 2_757
O4 P1 K1 133.40(11) . 2_757
O2 P1 K1 115.86(10) . 2_757
O1 P1 K1 59.41(10) . 2_757
O7 P2 O6 113.30(17) . .
O7 P2 O5 110.90(17) . .
O6 P2 O5 108.59(14) . .
O7 P2 O8 110.91(17) . .
O6 P2 O8 104.40(15) . .
O5 P2 O8 108.45(16) . .
O7 P2 K1 66.48(14) . 2_657
O6 P2 K1 113.05(11) . 2_657
O5 P2 K1 47.18(10) . 2_657
O8 P2 K1 140.13(11) . 2_657
P1 O1 Ru1 121.40(14) . 2_657
P1 O1 K1 94.61(11) . 2_757
Ru1 O1 K1 123.84(11) 2_657 2_757
P1 O1 K1 91.45(11) . .
Ru1 O1 K1 101.57(10) 2_657 .
K1 O1 K1 120.50(8) 2_757 .
P1 O2 Ru1 121.42(14) . .
P1 O3 K1 105.26(13) . 2_757
P1 O4 Cu1 130.86(16) . .
P1 O4 K1 109.93(13) . .
Cu1 O4 K1 118.77(11) . .
P2 O5 Ru1 120.62(15) . .
P2 O5 K1 110.12(13) . 2_657
Ru1 O5 K1 108.94(11) . 2_657
P2 O6 Ru1 121.10(15) . 2_657
P2 O8 K1 129.56(15) . 2_757
P2 O8 H1 112(4) . .
K1 O8 H1 117(4) 2_757 .
Ru1 O9 H9B 109.3 . .
Ru1 O9 H9C 109.3 . .
H9B O9 H9C 109.5 . .
Cu1 O10 H10A 109.4 . .
Cu1 O10 H10B 109.4 . .
H10A O10 H10B 109.5 . .
Cu1 O11 H11A 109.2 . .
Cu1 O11 H11B 109.5 . .
H11A O11 H11B 109.5 . .
K1 O12 H12A 109.3 . .
K1 O12 H12B 109.4 . .
H12A O12 H12B 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 O2 1.972(3) .
Ru1 O1 1.976(3) 2_657
Ru1 O5 1.988(3) .
Ru1 O6 1.998(3) 2_657
Ru1 O9 2.262(3) .
Ru1 Ru1 2.3531(5) 2_657
Ru1 K1 4.0611(12) 2_657
Cu1 O4 1.953(2) .
Cu1 O4 1.953(2) 2_756
Cu1 O10 2.059(3) .
Cu1 O10 2.059(3) 2_756
Cu1 O11 2.312(3) .
Cu1 O11 2.312(3) 2_756
K1 O4 2.757(3) .
K1 O8 2.805(3) 2_757
K1 O12 2.824(4) .
K1 O3 2.843(3) 2_757
K1 O5 2.954(3) 2_657
K1 O1 3.073(3) 2_757
K1 O1 3.174(3) .
K1 P1 3.5583(14) 2_757
K1 P2 3.7821(15) 2_657
P1 O3 1.518(3) .
P1 O4 1.519(3) .
P1 O2 1.562(3) .
P1 O1 1.564(3) .
P2 O7 1.488(3) .
P2 O6 1.549(3) .
P2 O5 1.554(3) .
P2 O8 1.566(3) .
O8 H1 0.84(2) .
O9 H9B 0.8500 .
O9 H9C 0.8500 .
O10 H10A 0.8500 .
O10 H10B 0.8500 .
O11 H11A 0.8501 .
O11 H11B 0.8500 .
O12 H12A 0.8500 .
O12 H12B 0.8500 .
