#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/17/4321719.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_4321719
loop_
_publ_author_name
'Wa-Hung Leung'
'Eddie Y. Y. Chan'
'Wing-Tak Wong'
_publ_section_title
;
 Synthesis and Electrochemistry of Ruthenium Complexes with an Oxygen
 Tripod Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              136
_journal_page_last               143
_journal_paper_doi               10.1021/ic980196s
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C36 H54 B Co F4 O12 P4 Ru'
_chemical_formula_weight         1049.52
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             'Wed Sep 23 11:52:05 1998'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                109.05(2)
_cell_angle_beta                 90.02(1)
_cell_angle_gamma                89.39(2)
_cell_formula_units_Z            2
_cell_length_a                   13.686(2)
_cell_length_b                   14.733(4)
_cell_length_c                   12.445(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    301.2
_cell_measurement_theta_max      16.6
_cell_measurement_theta_min      13.2
_cell_volume                     2371.8(9)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_diffrn_ambient_temperature      298
_diffrn_measurement_device       AFC7R
_diffrn_measurement_method       'omega/2-theta scans'
_diffrn_orient_matrix_UB_11      -0.01342
_diffrn_orient_matrix_UB_12      -0.05710
_diffrn_orient_matrix_UB_13      -0.06827
_diffrn_orient_matrix_UB_21      0.00289
_diffrn_orient_matrix_UB_22      -0.04243
_diffrn_orient_matrix_UB_23      0.04838
_diffrn_orient_matrix_UB_31      -0.07177
_diffrn_orient_matrix_UB_32      0.00978
_diffrn_orient_matrix_UB_33      0.01500
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  3.39
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6512
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2
_diffrn_standards_decay_%        -2.05
_diffrn_standards_interval_count 250
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.872
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.724
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   psi-scan
_exptl_crystal_colour            pale
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_description       plate
_exptl_crystal_F_000             1076.00
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.76
_refine_diff_density_min         -0.39
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   2.273
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         3153
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0480
_refine_ls_shift/esd_max         0.0420
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0551
_reflns_number_observed          3153
_reflns_number_total             6200
_reflns_observed_criterion       3.00
_cod_data_source_file            ic980196s_4.cif
_cod_data_source_block           wong502_WHL176A_Ru_22_May_Compound4
_cod_original_cell_volume        2372.0(9)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C36 H54 B Co F4 O12 P4 Ru '
_cod_database_code               4321719
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
'   -x,   -y,   -z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
Ru(1) 0.22591(8) 0.31939(7) 0.85348(9) 0.0559(3) Uij ? ?
Co(1) 0.2443(1) 0.1498(1) 1.0461(2) 0.0805(7) Uij ? ?
P(1) 0.2668(3) 0.3026(3) 1.1102(3) 0.073(1) Uij ? ?
P(2) 0.1168(3) 0.1670(3) 0.9528(3) 0.076(1) Uij ? ?
P(3) 0.3386(3) 0.1366(3) 0.9015(3) 0.080(1) Uij ? ?
P(4) 0.1903(2) 0.2868(2) 0.6653(3) 0.061(1) Uij ? ?
F(1) 0.6628(10) 0.359(1) 0.730(2) 0.340(10) Uij ? ?
F(2) 0.612(1) 0.2253(8) 0.644(1) 0.259(8) Uij ? ?
F(3) 0.5207(8) 0.3398(8) 0.742(1) 0.203(6) Uij ? ?
F(4) 0.592(1) 0.335(1) 0.588(2) 0.31(1) Uij ? ?
O(1) 0.0922(8) 0.4880(7) 0.9149(10) 0.129(5) Uij ? ?
O(2) 0.3470(6) 0.3991(5) 0.8364(7) 0.078(3) Uij ? ?
O(3) 0.2704(7) 0.3576(5) 1.0280(6) 0.084(3) Uij ? ?
O(4) 0.1169(5) 0.2345(6) 0.8850(7) 0.074(3) Uij ? ?
O(5) 0.3182(5) 0.1963(6) 0.8262(6) 0.070(3) Uij ? ?
O(6) 0.3642(10) 0.3254(8) 1.181(1) 0.142(6) Uij ? ?
O(7) 0.1857(8) 0.3481(7) 1.2018(8) 0.111(4) Uij ? ?
O(8) 0.0806(9) 0.0661(7) 0.8704(9) 0.133(5) Uij ? ?
O(9) 0.0257(8) 0.1961(9) 1.0352(9) 0.120(5) Uij ? ?
O(10) 0.337(1) 0.0262(7) 0.8251(10) 0.144(5) Uij ? ?
O(11) 0.4498(8) 0.1521(9) 0.9398(9) 0.123(5) Uij ? ?
O(12) 0.644(1) 0.459(1) 0.965(1) 0.224(7) Uij ? ?
C(1) 0.145(1) 0.4248(10) 0.889(1) 0.078(5) Uij ? ?
C(2) 0.250(3) 0.009(1) 1.047(2) 0.13(1) Uij ? ?
C(3) 0.171(2) 0.050(2) 1.098(3) 0.15(1) Uij ? ?
C(4) 0.196(3) 0.125(2) 1.191(3) 0.15(1) Uij ? ?
C(5) 0.294(4) 0.133(3) 1.193(3) 0.20(2) Uij ? ?
C(6) 0.331(2) 0.058(3) 1.099(3) 0.14(1) Uij ? ?
C(7) 0.439(2) 0.386(2) 1.189(2) 0.18(1) Uij ? ?
C(8) 0.523(2) 0.370(2) 1.241(2) 0.27(2) Uij ? ?
C(9) 0.154(1) 0.444(1) 1.241(1) 0.118(7) Uij ? ?
C(10) 0.078(1) 0.457(1) 1.326(1) 0.131(8) Uij ? ?
C(11) 0.068(2) 0.035(2) 0.762(2) 0.21(1) Uij ? ?
C(12) 0.040(2) -0.033(2) 0.691(2) 0.31(2) Uij ? ?
C(13) -0.059(2) 0.246(2) 1.024(2) 0.19(1) Uij ? ?
C(14) -0.130(2) 0.256(2) 1.095(2) 0.20(1) Uij ? ?
C(15) 0.362(2) -0.020(1) 0.721(2) 0.161(10) Uij ? ?
C(16) 0.360(2) -0.122(1) 0.684(2) 0.21(1) Uij ? ?
C(17) 0.523(1) 0.182(2) 0.888(2) 0.18(1) Uij ? ?
C(18) 0.617(1) 0.200(1) 0.937(2) 0.17(1) Uij ? ?
C(19) 0.244(1) 0.1741(10) 0.572(1) 0.078(5) Uij ? ?
C(20) 0.188(1) 0.099(1) 0.508(1) 0.106(6) Uij ? ?
C(21) 0.232(2) 0.016(2) 0.437(2) 0.16(1) Uij ? ?
C(22) 0.325(2) 0.002(2) 0.430(2) 0.18(1) Uij ? ?
C(23) 0.386(2) 0.077(2) 0.492(2) 0.17(1) Uij ? ?
C(24) 0.347(1) 0.163(1) 0.567(1) 0.112(7) Uij ? ?
C(25) 0.0598(9) 0.2814(8) 0.625(1) 0.069(5) Uij ? ?
C(26) -0.013(1) 0.277(1) 0.698(1) 0.094(6) Uij ? ?
C(27) -0.110(1) 0.272(1) 0.664(2) 0.122(8) Uij ? ?
C(28) -0.133(1) 0.271(1) 0.558(2) 0.128(9) Uij ? ?
C(29) -0.064(1) 0.276(1) 0.487(2) 0.113(7) Uij ? ?
C(30) 0.035(1) 0.281(1) 0.516(1) 0.092(6) Uij ? ?
C(31) 0.2354(9) 0.381(1) 0.611(1) 0.066(5) Uij ? ?
C(32) 0.199(1) 0.471(1) 0.654(1) 0.112(7) Uij ? ?
C(33) 0.229(2) 0.548(1) 0.622(2) 0.134(9) Uij ? ?
C(34) 0.294(2) 0.535(2) 0.543(2) 0.14(1) Uij ? ?
C(35) 0.337(2) 0.451(2) 0.499(2) 0.16(1) Uij ? ?
C(36) 0.306(1) 0.370(1) 0.529(1) 0.127(8) Uij ? ?
B(1) 0.595(2) 0.310(2) 0.674(3) 0.119(8) Uij ? ?
H(1) 0.2524 -0.0469 0.9817 0.1589 Uij ? ?
H(2) 0.1065 0.0305 1.0745 0.1761 Uij ? ?
H(3) 0.1520 0.1646 1.2453 0.1825 Uij ? ?
H(4) 0.3311 0.1808 1.2477 0.2357 Uij ? ?
H(5) 0.3978 0.0453 1.0773 0.1670 Uij ? ?
H(6) 0.1189 0.1036 0.5120 0.1271 Uij ? ?
H(7) 0.1912 -0.0333 0.3915 0.1947 Uij ? ?
H(8) 0.3515 -0.0570 0.3828 0.2136 Uij ? ?
H(9) 0.4548 0.0693 0.4833 0.2040 Uij ? ?
H(10) 0.3882 0.2116 0.6129 0.1341 Uij ? ?
H(11) 0.0033 0.2775 0.7723 0.1126 Uij ? ?
H(12) -0.1602 0.2682 0.7149 0.1463 Uij ? ?
H(13) -0.1993 0.2671 0.5354 0.1536 Uij ? ?
H(14) -0.0816 0.2764 0.4128 0.1353 Uij ? ?
H(15) 0.0839 0.2844 0.4632 0.1107 Uij ? ?
H(16) 0.1486 0.4830 0.7097 0.1349 Uij ? ?
H(17) 0.2011 0.6102 0.6572 0.1606 Uij ? ?
H(18) 0.3116 0.5863 0.5172 0.1684 Uij ? ?
H(19) 0.3900 0.4438 0.4468 0.1939 Uij ? ?
H(20) 0.3331 0.3086 0.4908 0.1519 Uij ? ?
H(21) 0.4559 0.3828 1.1136 0.2120 Uij ? ?
H(22) 0.4164 0.4488 1.2300 0.2120 Uij ? ?
H(23) 0.2078 0.4834 1.2736 0.1419 Uij ? ?
H(24) 0.1291 0.4607 1.1790 0.1419 Uij ? ?
H(25) 0.0244 0.0828 0.7521 0.2573 Uij ? ?
H(26) 0.1304 0.0421 0.7347 0.2573 Uij ? ?
H(27) -0.0401 0.3086 1.0277 0.2271 Uij ? ?
H(28) -0.0849 0.2134 0.9504 0.2271 Uij ? ?
H(29) 0.3186 -0.0001 0.6733 0.1933 Uij ? ?
H(30) 0.4264 -0.0021 0.7110 0.1933 Uij ? ?
H(31) 0.5318 0.1347 0.8154 0.2124 Uij ? ?
H(32) 0.5017 0.2406 0.8783 0.2124 Uij ? ?
H(33) 0.5095 0.3736 1.3169 0.3252 Uij ? ?
H(34) 0.5491 0.3078 1.2004 0.3252 Uij ? ?
H(35) 0.5705 0.4169 1.2407 0.3252 Uij ? ?
H(36) 0.0563 0.5221 1.3495 0.1572 Uij ? ?
H(37) 0.0253 0.4160 1.2943 0.1572 Uij ? ?
H(38) 0.1037 0.4424 1.3893 0.1572 Uij ? ?
H(39) -0.0213 -0.0517 0.7127 0.3783 Uij ? ?
H(40) 0.0332 -0.0197 0.6220 0.3783 Uij ? ?
H(41) 0.0862 -0.0840 0.6812 0.3783 Uij ? ?
H(42) -0.1096 0.2931 1.1688 0.2456 Uij ? ?
H(43) -0.1837 0.2881 1.0727 0.2456 Uij ? ?
H(44) -0.1510 0.1948 1.0952 0.2456 Uij ? ?
H(45) 0.2953 -0.1432 0.6891 0.2494 Uij ? ?
H(46) 0.3821 -0.1469 0.6076 0.2494 Uij ? ?
H(47) 0.4019 -0.1451 0.7310 0.2494 Uij ? ?
H(48) 0.6408 0.1435 0.9503 0.2090 Uij ? ?
H(49) 0.6600 0.2171 0.8879 0.2090 Uij ? ?
H(50) 0.6127 0.2507 1.0078 0.2090 Uij ? ?
H(51) 0.4024 0.3679 0.7784 0.1113 Uij ? ?
H(52) 0.3648 0.4660 0.8734 0.1113 Uij ? ?
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ru 0 2 -1.259 0.836 'International Tables'
P 0 8 0.102 0.094 'International Tables'
O 0 24 0.011 0.006 'International Tables'
C 0 72 0.003 0.002 'International Tables'
H 0 108 0.000 0.000 'International Tables'
Co 0 2 0.349 0.972 'International Tables'
F 0 8 0.017 0.010 'International Tables'
B 0 2 0.001 0.001 'International Tables'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
-4 -2 0
-4 -2 -1
-2 1 -4
