#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:39:36 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179758 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/54/7005443.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_7005443
loop_
_publ_author_name
'Baca, Svetlana G.'
'Adams, Harry'
'Sykes, Daniel'
'Faulkner, Stephen'
'Ward, Michael D.'
_publ_section_title
;
 Three-component coordination networks based on [Ru(phen)(CN)4]2?
 anions, near-infrared luminescent lanthanide(iii) cations, and
 ancillary oligopyridine ligands: structures and photophysical
 properties
;
_journal_issue                   23
_journal_name_full               'Dalton Transactions'
_journal_page_first              2419
_journal_paper_doi               10.1039/b702235b
_journal_year                    2007
_chemical_formula_sum            'C116 H110 K2 N32 O19 Pr2 Ru4'
_chemical_formula_weight         3020.66
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 100.91(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.400(3)
_cell_length_b                   28.050(6)
_cell_length_c                   17.400(4)
_cell_measurement_temperature    173(2)
_cell_volume                     6901(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX2 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  0.0781
_diffrn_reflns_av_sigmaI/netI    0.0474
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            94220
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    1.249
_exptl_absorpt_correction_T_max  0.8545
_exptl_absorpt_correction_T_min  0.6550
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3028
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.862
_refine_diff_density_min         -1.185
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     849
_refine_ls_number_reflns         12161
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.168
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_gt           0.0585
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0980P)²+32.0723P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1734
_refine_ls_wR_factor_ref         0.2070
_reflns_number_gt                8941
_reflns_number_total             12161
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b702235b.txt
_cod_data_source_block           imw772r
_cod_original_cell_volume        6901(2)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7005443
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pr1 Pr 0.76314(3) 0.020493(14) 0.14790(3) 0.03405(15) Uani 1 1 d . . .
Ru1 Ru 0.43099(4) 0.12448(2) 0.03460(4) 0.03752(19) Uani 1 1 d . . .
Ru2 Ru 0.93047(5) -0.13196(2) 0.32482(4) 0.0442(2) Uani 1 1 d . . .
K1A K 0.4870(4) 0.0097(3) 0.5726(5) 0.0565(13) Uani 0.30 1 d PU . 1
K1B K 0.4086(3) -0.01025(16) 0.5002(3) 0.0471(9) Uani 0.40 1 d PU . 2
K1C K 0.3675(4) 0.0087(2) 0.4135(4) 0.0394(11) Uani 0.30 1 d PU . 3
C1 C 0.2399(6) 0.1658(3) -0.0576(5) 0.0433(19) Uani 1 1 d . . .
H1 H 0.2264 0.1345 -0.0776 0.052 Uiso 1 1 calc R . .
C2 C 0.1749(6) 0.2020(3) -0.0826(5) 0.051(2) Uani 1 1 d . . .
H2 H 0.1185 0.1953 -0.1191 0.062 Uiso 1 1 calc R . .
C3 C 0.1928(7) 0.2471(4) -0.0543(6) 0.059(3) Uani 1 1 d . . .
H3 H 0.1487 0.2719 -0.0712 0.071 Uiso 1 1 calc R . .
C4 C 0.2750(6) 0.2570(3) -0.0008(6) 0.052(2) Uani 1 1 d . . .
C5 C 0.2998(9) 0.3030(4) 0.0360(7) 0.069(3) Uani 1 1 d . . .
H5 H 0.2576 0.3290 0.0227 0.083 Uiso 1 1 calc R . .
C6 C 0.3792(9) 0.3100(3) 0.0875(8) 0.074(3) Uani 1 1 d . . .
H6 H 0.3917 0.3406 0.1106 0.089 Uiso 1 1 calc R . .
C7 C 0.4471(8) 0.2721(3) 0.1093(7) 0.067(3) Uani 1 1 d . . .
C8 C 0.5294(9) 0.2767(4) 0.1642(9) 0.091(4) Uani 1 1 d . . .
H8 H 0.5445 0.3062 0.1906 0.109 Uiso 1 1 calc R . .
C9 C 0.5897(8) 0.2383(4) 0.1803(8) 0.082(4) Uani 1 1 d . . .
H9 H 0.6477 0.2413 0.2166 0.099 Uiso 1 1 calc R . .
C10 C 0.5649(6) 0.1950(4) 0.1431(7) 0.067(3) Uani 1 1 d . . .
H10 H 0.6068 0.1687 0.1551 0.080 Uiso 1 1 calc R . .
C11 C 0.4248(6) 0.2266(3) 0.0755(6) 0.049(2) Uani 1 1 d . . .
C12 C 0.3380(6) 0.2189(3) 0.0210(6) 0.048(2) Uani 1 1 d . . .
C13 C 0.5450(6) 0.0862(3) 0.0732(5) 0.0424(19) Uani 1 1 d . . .
C14 C 0.3653(5) 0.0685(3) -0.0178(5) 0.0427(19) Uani 1 1 d . . .
C15 C 0.4842(6) 0.1379(3) -0.0640(6) 0.053(2) Uani 1 1 d . . .
C16 C 0.3817(6) 0.1088(3) 0.1345(6) 0.050(2) Uani 1 1 d . . .
C17 C 0.7422(7) -0.1822(3) 0.2474(6) 0.054(2) Uani 1 1 d . . .
H17 H 0.7237 -0.1525 0.2230 0.064 Uiso 1 1 calc R . .
C18 C 0.6808(8) -0.2213(4) 0.2301(7) 0.072(3) Uani 1 1 d . . .
H18 H 0.6223 -0.2181 0.1946 0.086 Uiso 1 1 calc R . .
C19 C 0.7075(10) -0.2646(4) 0.2661(8) 0.079(4) Uani 1 1 d . . .
H19 H 0.6675 -0.2917 0.2546 0.095 Uiso 1 1 calc R . .
C20 C 0.7921(9) -0.2685(3) 0.3188(8) 0.069(3) Uani 1 1 d . . .
C21 C 0.8281(12) -0.3131(4) 0.3610(9) 0.085(4) Uani 1 1 d . . .
H21 H 0.7938 -0.3420 0.3498 0.102 Uiso 1 1 calc R . .
C22 C 0.9081(12) -0.3128(4) 0.4144(9) 0.087(4) Uani 1 1 d . . .
H22 H 0.9286 -0.3416 0.4409 0.104 Uiso 1 1 calc R . .
C23 C 0.9628(9) -0.2718(4) 0.4327(7) 0.074(4) Uani 1 1 d . . .
C24 C 1.0439(11) -0.2696(5) 0.4907(7) 0.086(4) Uani 1 1 d . . .
H24 H 1.0637 -0.2969 0.5219 0.103 Uiso 1 1 calc R . .
C25 C 1.0954(10) -0.2284(5) 0.5031(7) 0.084(4) Uani 1 1 d . . .
H25 H 1.1512 -0.2271 0.5422 0.100 Uiso 1 1 calc R . .
C26 C 1.0652(9) -0.1879(4) 0.4576(6) 0.074(3) Uani 1 1 d . . .
H26 H 1.1021 -0.1597 0.4662 0.089 Uiso 1 1 calc R . .
C27 C 0.9351(8) -0.2285(3) 0.3901(6) 0.062(3) Uani 1 1 d . . .
C28 C 0.8481(8) -0.2278(3) 0.3327(6) 0.059(3) Uani 1 1 d . . .
C29 C 0.8703(6) -0.0854(3) 0.2469(5) 0.0372(17) Uani 1 1 d . . .
C30 C 0.8580(7) -0.1035(3) 0.4039(5) 0.051(2) Uani 1 1 d . . .
C31 C 1.0023(6) -0.1630(3) 0.2473(5) 0.0442(19) Uani 1 1 d . . .
C32 C 1.0367(8) -0.0864(4) 0.3587(6) 0.064(3) Uani 1 1 d . . .
C33 C 0.8600(7) 0.0191(3) 0.3486(5) 0.048(2) Uani 1 1 d . . .
H33 H 0.8296 -0.0111 0.3427 0.058 Uiso 1 1 calc R . .
C34 C 0.9174(9) 0.0292(4) 0.4202(6) 0.068(3) Uani 1 1 d . . .
H34 H 0.9244 0.0069 0.4619 0.082 Uiso 1 1 calc R . .
C35 C 0.9635(8) 0.0719(4) 0.4293(6) 0.069(3) Uani 1 1 d . . .
H35 H 1.0045 0.0792 0.4773 0.083 Uiso 1 1 calc R . .
C36 C 0.9504(7) 0.1052(3) 0.3674(5) 0.052(2) Uani 1 1 d . . .
C37 C 0.9941(8) 0.1517(4) 0.3726(6) 0.066(3) Uani 1 1 d . . .
H37 H 1.0408 0.1592 0.4173 0.079 Uiso 1 1 calc R . .
C38 C 0.9708(7) 0.1849(4) 0.3161(6) 0.061(3) Uani 1 1 d . . .
H38 H 0.9981 0.2158 0.3228 0.073 Uiso 1 1 calc R . .
C39 C 0.9039(6) 0.1733(3) 0.2449(5) 0.045(2) Uani 1 1 d . . .
C40 C 0.8743(6) 0.2071(3) 0.1868(6) 0.050(2) Uani 1 1 d . . .
H40 H 0.8982 0.2387 0.1923 0.060 Uiso 1 1 calc R . .
C41 C 0.8102(6) 0.1940(3) 0.1217(6) 0.048(2) Uani 1 1 d . . .
H41 H 0.7860 0.2169 0.0828 0.058 Uiso 1 1 calc R . .
C42 C 0.7807(6) 0.1458(3) 0.1132(5) 0.0428(19) Uani 1 1 d . . .
H42 H 0.7400 0.1365 0.0660 0.051 Uiso 1 1 calc R . .
C43 C 0.8672(5) 0.1265(3) 0.2349(5) 0.0342(17) Uani 1 1 d . . .
C44 C 0.8885(5) 0.0923(3) 0.2979(5) 0.0394(18) Uani 1 1 d . . .
C45 C 1.0149(5) 0.0150(3) 0.2041(5) 0.0393(18) Uani 1 1 d . . .
H45 H 0.9959 0.0020 0.2492 0.047 Uiso 1 1 calc R . .
C46 C 1.1117(6) 0.0199(3) 0.2052(6) 0.047(2) Uani 1 1 d . . .
H46 H 1.1568 0.0107 0.2499 0.056 Uiso 1 1 calc R . .
C47 C 1.1405(6) 0.0384(3) 0.1399(6) 0.050(2) Uani 1 1 d . . .
H47 H 1.2058 0.0424 0.1391 0.060 Uiso 1 1 calc R . .
C48 C 1.0713(6) 0.0512(3) 0.0743(5) 0.0410(19) Uani 1 1 d . . .
C49 C 1.0954(7) 0.0696(3) 0.0021(6) 0.050(2) Uani 1 1 d . . .
H49 H 1.1600 0.0729 -0.0019 0.060 Uiso 1 1 calc R . .
C50 C 1.0292(7) 0.0816(3) -0.0576(6) 0.048(2) Uani 1 1 d . . .
H50 H 1.0475 0.0941 -0.1033 0.058 Uiso 1 1 calc R . .
C51 C 0.9301(7) 0.0766(3) -0.0565(5) 0.044(2) Uani 1 1 d . . .
C52 C 0.8568(8) 0.0884(3) -0.1185(5) 0.059(3) Uani 1 1 d . . .
H52 H 0.8715 0.1026 -0.1644 0.071 Uiso 1 1 calc R . .
C53 C 0.7652(8) 0.0801(3) -0.1145(6) 0.057(2) Uani 1 1 d . . .
H53 H 0.7161 0.0876 -0.1574 0.068 Uiso 1 1 calc R . .
C54 C 0.7441(6) 0.0602(3) -0.0457(5) 0.048(2) Uani 1 1 d . . .
H54 H 0.6798 0.0541 -0.0433 0.058 Uiso 1 1 calc R . .
C55 C 0.9025(6) 0.0575(2) 0.0130(5) 0.0366(17) Uani 1 1 d . . .
C56 C 0.9760(5) 0.0455(2) 0.0789(5) 0.0352(17) Uani 1 1 d . . .
C57 C 0.5100(14) 0.2154(9) 0.4004(14) 0.185(10) Uani 1 1 d . . .
H57A H 0.5067 0.2279 0.3473 0.277 Uiso 1 1 calc R A 1
H57B H 0.4712 0.2353 0.4283 0.277 Uiso 1 1 calc R A 1
H57C H 0.4864 0.1826 0.3975 0.277 Uiso 1 1 calc R A 1
C58 C 0.2259(17) 0.1248(9) 0.3402(12) 0.169(10) Uani 1 1 d . . .
H58A H 0.2174 0.1591 0.3464 0.253 Uiso 1 1 calc R B 1
H58B H 0.2035 0.1077 0.3823 0.253 Uiso 1 1 calc R B 1
H58C H 0.1896 0.1144 0.2895 0.253 Uiso 1 1 calc R B 1
N1 N 0.3202(4) 0.1732(2) -0.0069(4) 0.0393(15) Uani 1 1 d . . .
N2 N 0.4852(5) 0.1888(3) 0.0915(5) 0.0519(19) Uani 1 1 d . . .
N3 N 0.6147(5) 0.0658(3) 0.0951(5) 0.0513(19) Uani 1 1 d . . .
N4 N 0.3211(5) 0.0365(2) -0.0491(5) 0.0485(18) Uani 1 1 d . . .
N5 N 0.5145(7) 0.1430(4) -0.1211(6) 0.079(3) Uani 1 1 d . . .
N6 N 0.3584(7) 0.1000(4) 0.1925(6) 0.078(3) Uani 1 1 d . . .
N7 N 0.8241(6) -0.1848(2) 0.2959(4) 0.0464(18) Uani 1 1 d . . .
N8 N 0.9867(6) -0.1875(3) 0.4028(5) 0.057(2) Uani 1 1 d . . .
N9 N 0.8332(5) -0.0572(2) 0.2016(4) 0.0376(15) Uani 1 1 d . . .
N10 N 0.8136(7) -0.0870(3) 0.4475(5) 0.061(2) Uani 1 1 d . . .
N11 N 1.0426(5) -0.1834(3) 0.2054(5) 0.0534(19) Uani 1 1 d . . .
N12 N 1.0998(8) -0.0606(4) 0.3796(6) 0.097(4) Uani 1 1 d . . .
N13 N 0.8446(5) 0.0487(2) 0.2876(4) 0.0383(15) Uani 1 1 d . . .
N14 N 0.8075(4) 0.1128(2) 0.1683(4) 0.0352(14) Uani 1 1 d . . .
N15 N 0.9475(4) 0.0274(2) 0.1438(4) 0.0344(14) Uani 1 1 d . . .
N16 N 0.8108(5) 0.0495(2) 0.0169(4) 0.0395(15) Uani 1 1 d . . .
O1 O 0.6489(5) -0.0017(3) 0.2307(5) 0.080(2) Uani 1 1 d . . .
H1B H 0.6598 -0.0296 0.2493 0.095 Uiso 1 1 d R . .
H1C H 0.5972 -0.0079 0.1998 0.095 Uiso 1 1 d R . .
O2 O 0.2196(16) 0.0170(7) 0.4420(13) 0.141(10) Uani 0.50 1 d P . .
O3 O 0.3658(11) 0.0556(6) 0.6476(11) 0.088(5) Uani 0.50 1 d P . .
O4 O 0.6156(13) 0.0001(6) 0.7385(13) 0.108(7) Uani 0.50 1 d P . .
O5 O 0.260(2) -0.0876(13) 0.5185(15) 0.218(19) Uani 0.50 1 d P . .
O6 O 0.7719(8) 0.2051(6) 0.8004(10) 0.093(7) Uani 0.50 1 d P . .
O7 O 0.5285(13) 0.1039(5) 0.7322(9) 0.086(5) Uani 0.50 1 d P . .
O8 O 0.6887(6) 0.1970(4) -0.0693(6) 0.108(3) Uani 1 1 d . . .
H8B H 0.6888 0.2040 -0.1170 0.130 Uiso 1 1 d R . .
H8C H 0.6635 0.2170 -0.0424 0.130 Uiso 1 1 d R . .
O9 O 0.634(3) 0.1458(12) 0.5433(13) 0.24(2) Uani 0.50 1 d P C 1
O10 O 0.709(2) 0.157(2) 0.3493(19) 0.31(3) Uani 0.50 1 d P D 1
O11 O 0.5262(8) 0.0234(4) 0.8748(7) 0.127(4) Uani 1 1 d . E 1
O12 O 0.7196(15) 0.1302(12) 0.6889(12) 0.180(14) Uani 0.50 1 d P F 1
O13 O 0.6119(11) 0.2163(5) 0.4437(10) 0.180(6) Uani 1 1 d . G 1
H13 H 0.6403 0.1988 0.4156 0.216 Uiso 1 1 d R G 1
O14 O 0.3263(18) 0.1144(9) 0.3438(9) 0.267(12) Uani 1 1 d . H 1
H14 H 0.3477 0.0989 0.3845 0.321 Uiso 1 1 d R H 1
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'
N N 0.0061 0.0033 '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'
K K 0.2009 0.2494 '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'
Pr Pr -0.2180 2.8214 '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 Pr1 N4 87.1(3) . 3_655 ?
O1 Pr1 N9 80.1(2) . . ?
N4 Pr1 N9 79.0(2) 3_655 . ?
O1 Pr1 N3 74.1(3) . . ?
N4 Pr1 N3 78.6(2) 3_655 . ?
N9 Pr1 N3 146.4(2) . . ?
O1 Pr1 N13 76.4(2) . . ?
N4 Pr1 N13 155.7(2) 3_655 . ?
N9 Pr1 N13 80.7(2) . . ?
N3 Pr1 N13 112.9(2) . . ?
O1 Pr1 N16 153.8(2) . . ?
N4 Pr1 N16 76.9(2) 3_655 . ?
N9 Pr1 N16 116.1(2) . . ?
N3 Pr1 N16 82.5(2) . . ?
N13 Pr1 N16 124.6(2) . . ?
O1 Pr1 N14 109.6(2) . . ?
N4 Pr1 N14 141.9(2) 3_655 . ?
N9 Pr1 N14 136.3(2) . . ?
N3 Pr1 N14 73.9(2) . . ?
N13 Pr1 N14 61.93(19) . . ?
N16 Pr1 N14 73.77(19) . . ?
O1 Pr1 N15 144.0(2) . . ?
N4 Pr1 N15 112.6(2) 3_655 . ?
N9 Pr1 N15 75.0(2) . . ?
N3 Pr1 N15 137.3(2) . . ?
N13 Pr1 N15 74.34(19) . . ?
N16 Pr1 N15 62.1(2) . . ?
N14 Pr1 N15 73.77(18) . . ?
C14 Ru1 C13 91.1(3) . . ?
C14 Ru1 C15 89.0(4) . . ?
C13 Ru1 C15 88.1(4) . . ?
C14 Ru1 C16 90.5(4) . . ?
C13 Ru1 C16 89.6(4) . . ?
C15 Ru1 C16 177.6(4) . . ?
C14 Ru1 N1 95.3(3) . . ?
C13 Ru1 N1 172.7(3) . . ?
C15 Ru1 N1 88.4(3) . . ?
C16 Ru1 N1 93.9(3) . . ?
C14 Ru1 N2 172.9(3) . . ?
C13 Ru1 N2 95.4(3) . . ?
C15 Ru1 N2 94.1(3) . . ?
C16 Ru1 N2 86.7(3) . . ?
N1 Ru1 N2 78.4(3) . . ?
C29 Ru2 C32 89.5(4) . . ?
C29 Ru2 C30 89.4(3) . . ?
C32 Ru2 C30 90.7(4) . . ?
C29 Ru2 C31 92.3(3) . . ?
C32 Ru2 C31 90.7(4) . . ?
C30 Ru2 C31 177.8(3) . . ?
C29 Ru2 N7 95.5(3) . . ?
C32 Ru2 N7 175.0(3) . . ?
C30 Ru2 N7 89.7(3) . . ?
C31 Ru2 N7 88.7(3) . . ?
C29 Ru2 N8 174.4(3) . . ?
C32 Ru2 N8 95.9(4) . . ?
C30 Ru2 N8 92.2(3) . . ?
C31 Ru2 N8 85.9(3) . . ?
N7 Ru2 N8 79.0(3) . . ?
K1A K1A O3 140.5(6) 3_656 . ?
K1A K1A O4 133.5(5) 3_656 . ?
O3 K1A O4 85.4(5) . . ?
K1B K1B O2 144.8(5) 3_656 . ?
K1B K1B O5 147.2(5) 3_656 . ?
O2 K1B O5 65.9(6) . . ?
K1B K1B O3 102.0(4) 3_656 . ?
O2 K1B O3 79.6(4) . . ?
O5 K1B O3 94.5(5) . . ?
O2 K1C O4 118.6(8) . 3_656 ?
O2 K1C K1C 125.7(7) . 3_656 ?
O4 K1C K1C 115.4(4) 3_656 3_656 ?
O2 K1C H14 82.5 . . ?
O4 K1C H14 85.7 3_656 . ?
K1C K1C H14 106.9 3_656 . ?
N1 C1 C2 122.7(8) . . ?
N1 C1 H1 118.6 . . ?
C2 C1 H1 118.6 . . ?
C3 C2 C1 119.5(9) . . ?
C3 C2 H2 120.2 . . ?
C1 C2 H2 120.2 . . ?
C2 C3 C4 120.5(8) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 H3 119.8 . . ?
C3 C4 C12 116.9(9) . . ?
C3 C4 C5 125.5(9) . . ?
C12 C4 C5 117.6(9) . . ?
C6 C5 C4 122.5(9) . . ?
C6 C5 H5 118.8 . . ?
C4 C5 H5 118.8 . . ?
C5 C6 C7 121.5(10) . . ?
C5 C6 H6 119.3 . . ?
C7 C6 H6 119.3 . . ?
C8 C7 C11 117.9(10) . . ?
C8 C7 C6 124.2(10) . . ?
C11 C7 C6 117.7(10) . . ?
C7 C8 C9 119.5(10) . . ?
C7 C8 H8 120.2 . . ?
C9 C8 H8 120.2 . . ?
C8 C9 C10 119.5(11) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
N2 C10 C9 122.8(10) . . ?
N2 C10 H10 118.6 . . ?
C9 C10 H10 118.6 . . ?
N2 C11 C7 121.9(9) . . ?
N2 C11 C12 117.4(7) . . ?
C7 C11 C12 120.6(9) . . ?
N1 C12 C4 123.0(9) . . ?
N1 C12 C11 117.0(8) . . ?
C4 C12 C11 120.0(8) . . ?
N3 C13 Ru1 176.2(7) . . ?
N4 C14 Ru1 175.9(7) . . ?
N5 C15 Ru1 176.4(9) . . ?
N6 C16 Ru1 176.7(8) . . ?
N7 C17 C18 123.0(10) . . ?
N7 C17 H17 118.5 . . ?
C18 C17 H17 118.5 . . ?
C19 C18 C17 118.5(12) . . ?
C19 C18 H18 120.7 . . ?
C17 C18 H18 120.7 . . ?
C20 C19 C18 120.1(10) . . ?
C20 C19 H19 119.9 . . ?
C18 C19 H19 119.9 . . ?
C19 C20 C28 117.3(10) . . ?
C19 C20 C21 125.0(11) . . ?
C28 C20 C21 117.8(12) . . ?
C22 C21 C20 120.7(11) . . ?
C22 C21 H21 119.7 . . ?
C20 C21 H21 119.7 . . ?
C21 C22 C23 122.7(12) . . ?
C21 C22 H22 118.7 . . ?
C23 C22 H22 118.7 . . ?
C24 C23 C22 124.2(11) . . ?
C24 C23 C27 116.6(12) . . ?
C22 C23 C27 119.2(13) . . ?
C25 C24 C23 120.5(10) . . ?
C25 C24 H24 119.7 . . ?
C23 C24 H24 119.7 . . ?
C24 C25 C26 119.5(13) . . ?
C24 C25 H25 120.2 . . ?
C26 C25 H25 120.2 . . ?
N8 C26 C25 122.7(13) . . ?
N8 C26 H26 118.7 . . ?
C25 C26 H26 118.7 . . ?
N8 C27 C23 122.6(11) . . ?
N8 C27 C28 118.2(8) . . ?
C23 C27 C28 119.2(11) . . ?
N7 C28 C20 123.4(11) . . ?
N7 C28 C27 116.3(9) . . ?
C20 C28 C27 120.3(10) . . ?
N9 C29 Ru2 178.5(7) . . ?
N10 C30 Ru2 177.8(9) . . ?
N11 C31 Ru2 175.8(7) . . ?
N12 C32 Ru2 178.4(10) . . ?
N13 C33 C34 124.7(8) . . ?
N13 C33 H33 117.7 . . ?
C34 C33 H33 117.7 . . ?
C35 C34 C33 118.6(9) . . ?
C35 C34 H34 120.7 . . ?
C33 C34 H34 120.7 . . ?
C34 C35 C36 120.1(9) . . ?
C34 C35 H35 120.0 . . ?
C36 C35 H35 120.0 . . ?
C44 C36 C35 117.1(8) . . ?
C44 C36 C37 119.0(9) . . ?
C35 C36 C37 123.9(9) . . ?
C38 C37 C36 122.2(9) . . ?
C38 C37 H37 118.9 . . ?
C36 C37 H37 118.9 . . ?
C37 C38 C39 120.0(9) . . ?
C37 C38 H38 120.0 . . ?
C39 C38 H38 120.0 . . ?
C40 C39 C43 119.1(8) . . ?
C40 C39 C38 121.9(8) . . ?
C43 C39 C38 118.9(8) . . ?
C41 C40 C39 119.0(8) . . ?
C41 C40 H40 120.5 . . ?
C39 C40 H40 120.5 . . ?
C40 C41 C42 118.9(8) . . ?
C40 C41 H41 120.5 . . ?
C42 C41 H41 120.5 . . ?
N14 C42 C41 123.1(8) . . ?
N14 C42 H42 118.5 . . ?
C41 C42 H42 118.5 . . ?
N14 C43 C39 121.8(7) . . ?
N14 C43 C44 117.9(6) . . ?
C39 C43 C44 120.1(7) . . ?
N13 C44 C36 122.9(8) . . ?
N13 C44 C43 117.7(7) . . ?
C36 C44 C43 119.3(7) . . ?
N15 C45 C46 124.1(8) . . ?
N15 C45 H45 118.0 . . ?
C46 C45 H45 118.0 . . ?
C47 C46 C45 118.7(8) . . ?
C47 C46 H46 120.7 . . ?
C45 C46 H46 120.7 . . ?
C46 C47 C48 119.0(8) . . ?
C46 C47 H47 120.5 . . ?
C48 C47 H47 120.5 . . ?
C56 C48 C47 118.3(8) . . ?
C56 C48 C49 119.1(8) . . ?
C47 C48 C49 122.6(8) . . ?
C50 C49 C48 121.0(8) . . ?
C50 C49 H49 119.5 . . ?
C48 C49 H49 119.5 . . ?
C49 C50 C51 122.6(8) . . ?
C49 C50 H50 118.7 . . ?
C51 C50 H50 118.7 . . ?
C52 C51 C50 124.9(9) . . ?
C52 C51 C55 116.5(8) . . ?
C50 C51 C55 118.6(8) . . ?
C53 C52 C51 121.3(9) . . ?
C53 C52 H52 119.4 . . ?
C51 C52 H52 119.4 . . ?
C52 C53 C54 118.9(9) . . ?
C52 C53 H53 120.6 . . ?
C54 C53 H53 120.6 . . ?
N16 C54 C53 122.8(9) . . ?
N16 C54 H54 118.6 . . ?
C53 C54 H54 118.6 . . ?
N16 C55 C51 121.9(8) . . ?
N16 C55 C56 119.8(7) . . ?
C51 C55 C56 118.3(7) . . ?
N15 C56 C48 122.7(7) . . ?
N15 C56 C55 116.8(7) . . ?
C48 C56 C55 120.4(7) . . ?
C1 N1 C12 117.4(7) . . ?
C1 N1 Ru1 128.9(6) . . ?
C12 N1 Ru1 113.7(6) . . ?
C10 N2 C11 118.2(8) . . ?
C10 N2 Ru1 128.2(6) . . ?
C11 N2 Ru1 113.5(6) . . ?
C13 N3 Pr1 177.4(8) . . ?
C14 N4 Pr1 164.3(7) . 3_655 ?
C17 N7 C28 117.6(8) . . ?
C17 N7 Ru2 129.2(6) . . ?
C28 N7 Ru2 113.2(7) . . ?
C26 N8 C27 118.1(9) . . ?
C26 N8 Ru2 129.2(7) . . ?
C27 N8 Ru2 112.6(7) . . ?
C29 N9 Pr1 159.7(6) . . ?
C33 N13 C44 116.6(7) . . ?
C33 N13 Pr1 122.0(5) . . ?
C44 N13 Pr1 120.4(5) . . ?
C42 N14 C43 117.8(7) . . ?
C42 N14 Pr1 123.1(5) . . ?
C43 N14 Pr1 118.8(5) . . ?
C45 N15 C56 117.3(7) . . ?
C45 N15 Pr1 122.6(5) . . ?
C56 N15 Pr1 120.1(5) . . ?
C54 N16 C55 118.5(7) . . ?
C54 N16 Pr1 120.5(6) . . ?
C55 N16 Pr1 120.7(5) . . ?
Pr1 O1 H1B 111.1 . . ?
Pr1 O1 H1C 106.5 . . ?
H1B O1 H1C 97.4 . . ?
K1C O2 K1B 34.6(4) . . ?
K1A O3 K1B 29.1(3) . . ?
K1C O4 K1A 41.9(4) 3_656 . ?
H8B O8 H8C 117.3 . . ?
C57 O13 H13 103.3 . . ?
C58 O14 H14 109.9 . . ?
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
Pr1 O1 2.463(7) . ?
Pr1 N4 2.489(7) 3_655 ?
Pr1 N9 2.506(6) . ?
Pr1 N3 2.508(7) . ?
Pr1 N13 2.614(7) . ?
Pr1 N16 2.631(7) . ?
Pr1 N14 2.675(6) . ?
Pr1 N15 2.676(6) . ?
Ru1 C14 1.966(8) . ?
Ru1 C13 1.971(8) . ?
Ru1 C15 2.042(11) . ?
Ru1 C16 2.046(10) . ?
Ru1 N1 2.121(6) . ?
Ru1 N2 2.133(7) . ?
Ru2 C29 1.963(8) . ?
Ru2 C32 1.996(11) . ?
Ru2 C30 2.041(10) . ?
Ru2 C31 2.043(9) . ?
Ru2 N7 2.122(8) . ?
Ru2 N8 2.124(7) . ?
K1A K1A 2.678(15) 3_656 ?
K1A O3 2.696(18) . ?
K1A O4 3.13(2) . ?
K1B K1B 2.695(8) 3_656 ?
K1B O2 2.82(3) . ?
K1B O5 3.10(4) . ?
K1B O3 3.31(2) . ?
K1C O2 2.29(2) . ?
K1C O4 2.71(2) 3_656 ?
K1C K1C 4.417(11) 3_656 ?
K1C H14 2.5849 . ?
C1 N1 1.331(10) . ?
C1 C2 1.394(12) . ?
C1 H1 0.9500 . ?
C2 C3 1.365(14) . ?
C2 H2 0.9500 . ?
C3 C4 1.388(14) . ?
C3 H3 0.9500 . ?
C4 C12 1.408(12) . ?
C4 C5 1.455(14) . ?
C5 C6 1.327(16) . ?
C5 H5 0.9500 . ?
C6 C7 1.446(15) . ?
C6 H6 0.9500 . ?
C7 C8 1.380(17) . ?
C7 C11 1.419(12) . ?
C8 C9 1.381(17) . ?
C8 H8 0.9500 . ?
C9 C10 1.391(13) . ?
C9 H9 0.9500 . ?
C10 N2 1.328(12) . ?
C10 H10 0.9500 . ?
C11 N2 1.366(11) . ?
C11 C12 1.435(13) . ?
C12 N1 1.377(10) . ?
C13 N3 1.154(10) . ?
C14 N4 1.173(10) . ?
C15 N5 1.168(13) . ?
C16 N6 1.150(12) . ?
C17 N7 1.317(12) . ?
C17 C18 1.405(13) . ?
C17 H17 0.9500 . ?
C18 C19 1.389(16) . ?
C18 H18 0.9500 . ?
C19 C20 1.384(17) . ?
C19 H19 0.9500 . ?
C20 C28 1.394(14) . ?
C20 C21 1.492(16) . ?
C21 C22 1.336(19) . ?
C21 H21 0.9500 . ?
C22 C23 1.395(18) . ?
C22 H22 0.9500 . ?
C23 C24 1.393(18) . ?
C23 C27 1.439(13) . ?
C24 C25 1.368(19) . ?
C24 H24 0.9500 . ?
C25 C26 1.405(15) . ?
C25 H25 0.9500 . ?
C26 N8 1.333(14) . ?
C26 H26 0.9500 . ?
C27 N8 1.365(14) . ?
C27 C28 1.447(16) . ?
C28 N7 1.377(11) . ?
C29 N9 1.171(10) . ?
C30 N10 1.175(12) . ?
C31 N11 1.164(11) . ?
C32 N12 1.164(13) . ?
C33 N13 1.333(10) . ?
C33 C34 1.386(13) . ?
C33 H33 0.9500 . ?
C34 C35 1.364(15) . ?
C34 H34 0.9500 . ?
C35 C36 1.411(14) . ?
C35 H35 0.9500 . ?
C36 C44 1.408(12) . ?
C36 C37 1.443(13) . ?
C37 C38 1.349(14) . ?
C37 H37 0.9500 . ?
C38 C39 1.455(13) . ?
C38 H38 0.9500 . ?
C39 C40 1.392(12) . ?
C39 C43 1.415(10) . ?
C40 C41 1.369(13) . ?
C40 H40 0.9500 . ?
C41 C42 1.417(11) . ?
C41 H41 0.9500 . ?
C42 N14 1.336(10) . ?
C42 H42 0.9500 . ?
C43 N14 1.361(10) . ?
C43 C44 1.446(11) . ?
C44 N13 1.372(10) . ?
C45 N15 1.333(10) . ?
C45 C46 1.397(11) . ?
C45 H45 0.9500 . ?
C46 C47 1.382(13) . ?
C46 H46 0.9500 . ?
C47 C48 1.412(13) . ?
C47 H47 0.9500 . ?
C48 C56 1.399(11) . ?
C48 C49 1.460(12) . ?
C49 C50 1.314(13) . ?
C49 H49 0.9500 . ?
C50 C51 1.437(13) . ?
C50 H50 0.9500 . ?
C51 C52 1.400(13) . ?
C51 C55 1.447(11) . ?
C52 C53 1.354(14) . ?
C52 H52 0.9500 . ?
C53 C54 1.406(13) . ?
C53 H53 0.9500 . ?
C54 N16 1.343(10) . ?
C54 H54 0.9500 . ?
C55 N16 1.354(10) . ?
C55 C56 1.446(11) . ?
C56 N15 1.369(10) . ?
C57 O13 1.52(2) . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 O14 1.46(3) . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
N4 Pr1 2.489(7) 3_655 ?
O1 H1B 0.8500 . ?
O1 H1C 0.8497 . ?
O4 K1C 2.71(2) 3_656 ?
O8 H8B 0.8534 . ?
O8 H8C 0.8534 . ?
O13 H13 0.8494 . ?
O14 H14 0.8400 . ?
