#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:59:06 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179498 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/95/4339541.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_4339541
loop_
_publ_author_name
'Liu, Bin'
'Li, Bao-Long'
'Li, Yi-Zhi'
'Chen, Yu'
'Bao, Song-Song'
'Zheng, Li-Min'
_publ_section_title
;
 Lanthanide diruthenium(II,III) compounds showing layered and PtS-type
 open framework structures.
;
_journal_issue                   21
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8524
_journal_page_last               8532
_journal_paper_doi               10.1021/ic0621695
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C4 H20 Ho O20 P4 Ru2, 8(H2 O)'
_chemical_formula_sum            'C4 H36 Ho O28 P4 Ru2'
_chemical_formula_weight         1023.28
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.146(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.495(18)
_cell_length_b                   14.45(2)
_cell_length_c                   15.39(2)
_cell_measurement_reflns_used    881
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.13
_cell_measurement_theta_min      2.65
_cell_volume                     2771(7)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart Apex CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_sigmaI/netI    0.0855
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7385
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    4.244
_exptl_absorpt_correction_T_max  0.6084
_exptl_absorpt_correction_T_min  0.4553
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker(2000)'
_exptl_crystal_colour            'red brown''
_exptl_crystal_density_diffrn    2.453
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1996
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.932
_refine_diff_density_min         -1.027
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2721
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0489
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0400P)²+0.2200P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0892
_reflns_number_gt                1958
_reflns_number_total             2721
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0621695-file010.cif
_cod_data_source_block           51029bm
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'C2/c  '
_cod_database_code               4339541
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ru1 Ru 0.66662(5) 0.21192(4) 0.49806(4) 0.03505(17) Uani 1 1 d .
Ho1 Ho 0.5000 0.50995(3) 0.2500 0.03367(15) Uani 1 2 d S
P1 P 0.80137(15) 0.15455(13) 0.35488(13) 0.0353(5) Uani 1 1 d .
P2 P 0.68513(16) 0.33801(14) 0.34546(13) 0.0351(4) Uani 1 1 d .
O1 O 0.7152(4) 0.1200(3) 0.4132(3) 0.0331(11) Uani 1 1 d .
O2 O 0.8911(4) 0.1992(3) 0.4138(3) 0.0287(10) Uani 1 1 d .
O3 O 0.8476(4) 0.0809(3) 0.3021(3) 0.0346(12) Uani 1 1 d .
O4 O 0.6009(4) 0.2936(3) 0.4019(3) 0.0309(11) Uani 1 1 d .
O5 O 0.7802(4) 0.3757(3) 0.4064(3) 0.0331(11) Uani 1 1 d .
O6 O 0.6381(4) 0.4096(3) 0.2859(3) 0.0337(11) Uani 1 1 d .
O7 O 0.8217(4) 0.2767(3) 0.2295(4) 0.0379(12) Uani 1 1 d .
H7C H 0.8721 0.2968 0.2644 0.046 Uiso 1 1 d R
O8 O 0.5106(4) 0.1334(3) 0.4961(3) 0.0306(11) Uani 1 1 d .
H8B H 0.4600 0.1697 0.5065 0.037 Uiso 1 1 d R
H8C H 0.4977 0.1102 0.4462 0.037 Uiso 1 1 d R
O9 O 0.5687(4) 0.6282(3) 0.3482(3) 0.0313(11) Uani 1 1 d .
H9A H 0.5365 0.6254 0.3943 0.038 Uiso 1 1 d R
H9C H 0.5581 0.6804 0.3250 0.038 Uiso 1 1 d R
O10 O 0.5325(4) 0.4482(4) 0.1110(3) 0.0373(12) Uani 1 1 d .
H10A H 0.4897 0.4036 0.1003 0.045 Uiso 1 1 d R
H10C H 0.5970 0.4299 0.1089 0.045 Uiso 1 1 d R
O11 O 0.0187(4) 0.4996(3) 0.1244(3) 0.0358(12) Uani 1 1 d .
H11D H 0.0862 0.4934 0.1219 0.043 Uiso 1 1 d R
H11B H -0.0020 0.4668 0.1651 0.043 Uiso 1 1 d R
O12 O 0.6956(4) 0.5420(3) 0.4994(4) 0.0425(14) Uani 1 1 d .
H12D H 0.6732 0.5302 0.4475 0.051 Uiso 1 1 d R
H12A H 0.7605 0.5247 0.5084 0.051 Uiso 1 1 d R
O13 O 0.8423(4) 0.4590(3) 0.2187(3) 0.0322(11) Uani 1 1 d .
H13D H 0.7782 0.4576 0.1955 0.039 Uiso 1 1 d R
H13B H 0.8587 0.5137 0.2330 0.039 Uiso 1 1 d R
O14 O 0.8093(4) 0.3072(3) 0.0424(3) 0.0339(12) Uani 1 1 d .
H14D H 0.7523 0.3345 0.0547 0.041 Uiso 1 1 d R
H14C H 0.8330 0.2746 0.0849 0.041 Uiso 1 1 d R
C1 C 0.7381(5) 0.2412(5) 0.2837(5) 0.0306(15) Uani 1 1 d .
C2 C 0.6513(7) 0.2022(5) 0.2210(5) 0.0383(18) Uani 1 1 d .
H2A H 0.6813 0.1527 0.1866 0.057 Uiso 1 1 calc R
H2B H 0.6230 0.2513 0.1819 0.057 Uiso 1 1 calc R
H2C H 0.5934 0.1772 0.2536 0.057 Uiso 1 1 calc R
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'
P P 0.1023 0.0942 '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'
Ho Ho -0.2175 4.6783 '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
O1 Ru1 O5 87.7(2) . 7_656
O1 Ru1 O4 92.1(2) . .
O5 Ru1 O4 174.97(19) 7_656 .
O1 Ru1 O2 176.41(19) . 7_656
O5 Ru1 O2 91.4(2) 7_656 7_656
O4 Ru1 O2 88.6(2) . 7_656
O1 Ru1 O8 87.7(2) . .
O5 Ru1 O8 86.2(2) 7_656 .
O4 Ru1 O8 88.8(2) . .
O2 Ru1 O8 88.79(19) 7_656 .
O1 Ru1 Ru1 90.98(16) . 7_656
O5 Ru1 Ru1 91.73(16) 7_656 7_656
O4 Ru1 Ru1 93.30(15) . 7_656
O2 Ru1 Ru1 92.51(15) 7_656 7_656
O8 Ru1 Ru1 177.57(13) . 7_656
O6 Ho1 O6 101.5(2) 2_655 .
O6 Ho1 O3 143.86(17) 2_655 4_655
O6 Ho1 O3 75.15(19) . 4_655
O6 Ho1 O3 75.15(19) 2_655 3_455
O6 Ho1 O3 143.86(17) . 3_455
O3 Ho1 O3 128.4(3) 4_655 3_455
O6 Ho1 O10 73.77(17) 2_655 .
O6 Ho1 O10 78.73(18) . .
O3 Ho1 O10 70.27(18) 4_655 .
O3 Ho1 O10 131.63(18) 3_455 .
O6 Ho1 O10 78.73(18) 2_655 2_655
O6 Ho1 O10 73.77(17) . 2_655
O3 Ho1 O10 131.63(18) 4_655 2_655
O3 Ho1 O10 70.27(18) 3_455 2_655
O10 Ho1 O10 135.9(3) . 2_655
O6 Ho1 O9 146.29(15) 2_655 .
O6 Ho1 O9 94.00(19) . .
O3 Ho1 O9 69.07(17) 4_655 .
O3 Ho1 O9 74.74(18) 3_455 .
O10 Ho1 O9 139.20(16) . .
O10 Ho1 O9 77.14(19) 2_655 .
O6 Ho1 O9 94.00(18) 2_655 2_655
O6 Ho1 O9 146.29(15) . 2_655
O3 Ho1 O9 74.74(18) 4_655 2_655
O3 Ho1 O9 69.07(17) 3_455 2_655
O10 Ho1 O9 77.14(19) . 2_655
O10 Ho1 O9 139.20(16) 2_655 2_655
O9 Ho1 O9 89.2(3) . 2_655
O3 P1 O2 109.2(3) . .
O3 P1 O1 113.9(3) . .
O2 P1 O1 107.8(3) . .
O3 P1 C1 109.6(3) . .
O2 P1 C1 109.7(3) . .
O1 P1 C1 106.6(3) . .
O6 P2 O4 112.5(3) . .
O6 P2 O5 112.4(3) . .
O4 P2 O5 109.1(3) . .
O6 P2 C1 110.7(3) . .
O4 P2 C1 105.0(3) . .
O5 P2 C1 106.8(3) . .
P1 O1 Ru1 115.3(3) . .
P1 O2 Ru1 112.4(3) . 7_656
P1 O3 Ho1 149.0(3) . 3_545
P2 O4 Ru1 113.3(3) . .
P2 O5 Ru1 114.6(3) . 7_656
P2 O6 Ho1 148.5(3) . .
C1 O7 H7C 106.6 . .
Ru1 O8 H8B 110.0 . .
Ru1 O8 H8C 108.8 . .
H8B O8 H8C 108.9 . .
Ho1 O9 H9A 109.0 . .
Ho1 O9 H9C 109.4 . .
H9A O9 H9C 109.3 . .
Ho1 O10 H10A 108.3 . .
Ho1 O10 H10C 112.0 . .
H10A O10 H10C 110.1 . .
H11D O11 H11B 109.5 . .
H12D O12 H12A 110.0 . .
H13D O13 H13B 109.7 . .
H14D O14 H14C 109.8 . .
O7 C1 C2 105.9(6) . .
O7 C1 P1 106.6(5) . .
C2 C1 P1 113.1(5) . .
O7 C1 P2 108.9(5) . .
C2 C1 P2 110.2(5) . .
P1 C1 P2 111.7(4) . .
C1 C2 H2A 109.5 . .
C1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
C1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 O1 1.989(5) .
Ru1 O5 2.017(5) 7_656
Ru1 O4 2.021(5) .
Ru1 O2 2.037(5) 7_656
Ru1 O8 2.254(5) .
Ru1 Ru1 2.353(3) 7_656
Ho1 O6 2.291(6) 2_655
Ho1 O6 2.291(6) .
Ho1 O3 2.353(5) 4_655
Ho1 O3 2.353(5) 3_455
Ho1 O10 2.379(6) .
Ho1 O10 2.379(6) 2_655
Ho1 O9 2.398(5) .
Ho1 O9 2.398(5) 2_655
P1 O3 1.481(5) .
P1 O2 1.532(6) .
P1 O1 1.534(5) .
P1 C1 1.808(8) .
P2 O6 1.475(6) .
P2 O4 1.550(5) .
P2 O5 1.557(6) .
P2 C1 1.841(7) .
O2 Ru1 2.037(5) 7_656
O3 Ho1 2.353(5) 3_545
O5 Ru1 2.017(5) 7_656
O7 C1 1.474(8) .
O7 H7C 0.8489 .
O8 H8B 0.8455 .
O8 H8C 0.8422 .
O9 H9A 0.8416 .
O9 H9C 0.8405 .
O10 H10A 0.8450 .
O10 H10C 0.8500 .
O11 H11D 0.8510 .
O11 H11B 0.8407 .
O12 H12D 0.8438 .
O12 H12A 0.8511 .
O13 H13D 0.8521 .
O13 H13B 0.8407 .
O14 H14D 0.8472 .
O14 H14C 0.8432 .
C1 C2 1.507(11) .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
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
O12 H12D O9 0.84 2.40 2.991(8) 127.7 .
O13 H13D O6 0.85 2.41 2.910(7) 117.7 .
O14 H14C O7 0.84 2.24 2.907(9) 136.0 .
O8 H8B O14 0.85 2.03 2.798(7) 151.0 8_456
O8 H8C O11 0.84 1.93 2.685(7) 147.9 4_545
O9 H9A O2 0.84 2.15 2.706(7) 123.7 3_455
O9 H9C O7 0.84 2.25 2.853(7) 128.5 4_655
O13 H13D O3 0.85 2.38 2.953(8) 125.2 4_655
O10 H10A O4 0.84 1.95 2.785(7) 169.1 2_655
O11 H11D O5 0.85 2.44 3.149(7) 140.7 2_655
O10 H10C O12 0.85 2.20 2.762(7) 123.9 6_565
O14 H14D O12 0.85 2.08 2.658(8) 125.0 6_565
O11 H11B O13 0.84 2.17 2.788(7) 130.2 1_455
O12 H12A O1 0.85 2.42 2.883(8) 114.7 7_656
