#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:18:19 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180071 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/17/7051769.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_7051769
loop_
_publ_author_name
'Wei, Qiao-Hua'
'Argent, Stephen P.'
'Adams, Harry'
'Ward, Michael D.'
_publ_section_title
;
 Post-coordination functionalisation of pyrazolyl-based ligands as a
 route to polynuclear complexes based on an inert RuIIN6 core
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              73
_journal_paper_doi               10.1039/b708572a
_journal_volume                  32
_journal_year                    2008
_chemical_formula_sum            'C86 H78 N24 O10 Ru'
_chemical_formula_weight         1708.79
_chemical_name_systematic
;
?
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.7252(5)
_cell_length_b                   16.7252(5)
_cell_length_c                   16.1385(10)
_cell_measurement_temperature    150(2)
_cell_volume                     4514.5(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-2 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  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            62954
_diffrn_reflns_theta_full        32.68
_diffrn_reflns_theta_max         32.68
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.242
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1772
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.026
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.133
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         8235
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0582
_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)+(0.1162P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1496
_refine_ls_wR_factor_ref         0.1532
_reflns_number_gt                7779
_reflns_number_total             8235
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b708572a.txt
_cod_data_source_block           RuL1
_cod_original_sg_symbol_H-M      I-4
_cod_database_code               7051769
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'y, -x, -z'
'-x, -y, z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+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
Ru1 Ru 0.0000 1.0000 1.0000 0.02924(8) Uani 1 4 d S . .
N11 N 0.1773(4) 0.6507(4) 0.6668(4) 0.1012(14) Uani 1 1 d . . .
C12 C 0.2166(3) 0.6175(2) 0.7316(3) 0.0744(12) Uani 1 1 d . . .
C13 C 0.2087(4) 0.5387(3) 0.7482(6) 0.105(2) Uani 1 1 d . . .
H13 H 0.2360 0.5150 0.7920 0.125 Uiso 1 1 calc R . .
C14 C 0.1560(4) 0.4921(4) 0.6950(6) 0.114(3) Uani 1 1 d . . .
H14 H 0.1494 0.4376 0.7039 0.137 Uiso 1 1 calc R . .
C15 C 0.1183(6) 0.5278(7) 0.6348(7) 0.139(3) Uani 1 1 d . . .
H15 H 0.0838 0.4980 0.6017 0.167 Uiso 1 1 calc R . .
C16 C 0.1282(9) 0.6117(6) 0.6178(8) 0.171(5) Uani 1 1 d . . .
H16 H 0.1014 0.6369 0.5746 0.205 Uiso 1 1 calc R . .
N21 N 0.28454(18) 0.74406(17) 0.7510(2) 0.0585(7) Uani 1 1 d . . .
N22 N 0.3350(2) 0.7779(2) 0.8081(3) 0.0720(9) Uani 1 1 d . . .
C23 C 0.3484(3) 0.7266(5) 0.8730(3) 0.097(2) Uani 1 1 d . . .
H23 H 0.3807 0.7370 0.9187 0.116 Uiso 1 1 calc R . .
C24 C 0.3091(4) 0.6621(3) 0.8605(3) 0.0875(17) Uani 1 1 d . . .
H24 H 0.3066 0.6176 0.8950 0.105 Uiso 1 1 calc R . .
C25 C 0.2692(2) 0.6724(2) 0.7815(2) 0.0611(8) Uani 1 1 d . . .
C31 C 0.3676(3) 0.8579(3) 0.7931(5) 0.105(2) Uani 1 1 d . . .
H31A H 0.3794 0.8636 0.7345 0.126 Uiso 1 1 calc R . .
H31B H 0.4175 0.8635 0.8232 0.126 Uiso 1 1 calc R . .
C32 C 0.3112(3) 0.9240(3) 0.8192(4) 0.0794(14) Uani 1 1 d . . .
C33 C 0.3120(2) 0.9437(3) 0.9081(3) 0.0780(13) Uani 1 1 d . . .
H33 H 0.3439 0.9161 0.9456 0.094 Uiso 1 1 calc R . .
C34 C 0.2626(2) 1.0057(2) 0.9325(3) 0.0650(9) Uani 1 1 d . . .
H34 H 0.2624 1.0208 0.9880 0.078 Uiso 1 1 calc R . .
C35 C 0.21309(18) 1.04638(17) 0.87731(19) 0.0487(6) Uani 1 1 d . . .
C36 C 0.2119(3) 1.0226(2) 0.7944(2) 0.0649(10) Uani 1 1 d . . .
H36 H 0.1780 1.0484 0.7573 0.078 Uiso 1 1 calc R . .
C37 C 0.2608(3) 0.9608(3) 0.7665(3) 0.0757(15) Uani 1 1 d . . .
H37 H 0.2586 0.9449 0.7113 0.091 Uiso 1 1 calc R . .
C38 C 0.16291(19) 1.11764(18) 0.9029(2) 0.0465(6) Uani 1 1 d . . .
H38A H 0.1891 1.1664 0.8851 0.056 Uiso 1 1 calc R . .
H38B H 0.1113 1.1148 0.8757 0.056 Uiso 1 1 calc R . .
N41 N 0.09787(11) 1.07199(11) 1.03014(13) 0.0331(3) Uani 1 1 d . . .
N42 N 0.15116(11) 1.12012(11) 0.9920(2) 0.0398(5) Uani 1 1 d . . .
C43 C 0.19891(16) 1.15758(17) 1.0481(2) 0.0496(6) Uani 1 1 d . . .
H43 H 0.2405 1.1926 1.0358 0.060 Uiso 1 1 calc R . .
C44 C 0.17551(17) 1.13513(19) 1.1251(2) 0.0470(6) Uani 1 1 d . . .
H44 H 0.1967 1.1516 1.1756 0.056 Uiso 1 1 calc R . .
C45 C 0.11173(14) 1.08111(15) 1.11191(15) 0.0384(4) Uani 1 1 d . . .
N51 N 0.0000 1.0000 1.12606(13) 0.0333(4) Uani 1 2 d S . .
C52 C 0.05738(15) 1.03933(16) 1.16782(15) 0.0400(4) Uani 1 1 d . . .
C53 C 0.0609(2) 1.0398(2) 1.25416(18) 0.0550(7) Uani 1 1 d . . .
H53 H 0.1020 1.0656 1.2823 0.066 Uiso 1 1 calc R . .
C54 C 0.0000 1.0000 1.29641(19) 0.0651(11) Uani 1 2 d S . .
H54 H 0.0000 1.0000 1.3540 0.078 Uiso 1 2 calc SR . .
O100 O 0.3157 1.2810 0.91267(19) 0.134(4) Uiso 0.50 1 d PR . .
O101 O 0.0601 0.3515 0.48854(19) 0.347(16) Uiso 0.50 1 d PR . .
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'
Ru Ru -1.2594 0.8363 '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
N51 Ru1 N51 180.0 2_467 . ?
N51 Ru1 N41 103.46(6) 2_467 . ?
N51 Ru1 N41 76.54(6) . . ?
N51 Ru1 N41 76.54(6) 2_467 4_667 ?
N51 Ru1 N41 103.46(6) . 4_667 ?
N41 Ru1 N41 93.11(3) . 4_667 ?
N51 Ru1 N41 103.46(6) 2_467 3_575 ?
N51 Ru1 N41 76.54(6) . 3_575 ?
N41 Ru1 N41 153.08(11) . 3_575 ?
N41 Ru1 N41 93.11(3) 4_667 3_575 ?
N51 Ru1 N41 76.54(6) 2_467 2_467 ?
N51 Ru1 N41 103.46(6) . 2_467 ?
N41 Ru1 N41 93.11(3) . 2_467 ?
N41 Ru1 N41 153.08(11) 4_667 2_467 ?
N41 Ru1 N41 93.11(3) 3_575 2_467 ?
C16 N11 C12 124.4(7) . . ?
C13 C12 N11 120.3(6) . . ?
C13 C12 C25 123.1(6) . . ?
N11 C12 C25 116.6(4) . . ?
C12 C13 C14 117.7(8) . . ?
C15 C14 C13 119.2(7) . . ?
C14 C15 C16 122.1(10) . . ?
N11 C16 C15 116.2(10) . . ?
C25 N21 N22 104.2(4) . . ?
N21 N22 C23 110.8(4) . . ?
N21 N22 C31 119.7(5) . . ?
C23 N22 C31 129.5(6) . . ?
C24 C23 N22 108.8(5) . . ?
C23 C24 C25 106.0(4) . . ?
N21 C25 C24 110.3(4) . . ?
N21 C25 C12 117.9(4) . . ?
C24 C25 C12 131.8(4) . . ?
N22 C31 C32 112.8(3) . . ?
C37 C32 C33 121.3(4) . . ?
C37 C32 C31 123.3(5) . . ?
C33 C32 C31 115.4(6) . . ?
C34 C33 C32 116.1(5) . . ?
C33 C34 C35 122.6(4) . . ?
C34 C35 C36 118.8(3) . . ?
C34 C35 C38 122.6(3) . . ?
C36 C35 C38 118.5(4) . . ?
C37 C36 C35 120.8(5) . . ?
C32 C37 C36 120.2(4) . . ?
N42 C38 C35 111.6(3) . . ?
C45 N41 N42 105.4(2) . . ?
C45 N41 Ru1 115.32(17) . . ?
N42 N41 Ru1 139.0(2) . . ?
N41 N42 C43 111.1(3) . . ?
N41 N42 C38 121.6(2) . . ?
C43 N42 C38 126.4(2) . . ?
C44 C43 N42 108.2(3) . . ?
C43 C44 C45 104.9(3) . . ?
N41 C45 C44 110.5(3) . . ?
N41 C45 C52 116.4(2) . . ?
C44 C45 C52 133.1(3) . . ?
C52 N51 C52 119.8(3) . 3_575 ?
C52 N51 Ru1 120.08(13) . . ?
C52 N51 Ru1 120.08(13) 3_575 . ?
N51 C52 C53 122.2(3) . . ?
N51 C52 C45 111.7(2) . . ?
C53 C52 C45 126.1(3) . . ?
C54 C53 C52 117.1(3) . . ?
C53 C54 C53 121.5(3) 3_575 . ?
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
Ru1 N51 2.034(2) 2_467 ?
Ru1 N51 2.034(2) . ?
Ru1 N41 2.0894(19) . ?
Ru1 N41 2.0894(19) 4_667 ?
Ru1 N41 2.0894(19) 3_575 ?
Ru1 N41 2.0894(19) 2_467 ?
N11 C16 1.313(10) . ?
N11 C12 1.355(8) . ?
C12 C13 1.352(7) . ?
C12 C25 1.504(7) . ?
C13 C14 1.456(12) . ?
C14 C15 1.304(13) . ?
C15 C16 1.440(14) . ?
N21 C25 1.321(5) . ?
N21 N22 1.371(5) . ?
N22 C23 1.374(8) . ?
N22 C31 1.464(7) . ?
C23 C24 1.280(9) . ?
C24 C25 1.449(7) . ?
C31 C32 1.514(6) . ?
C32 C37 1.346(8) . ?
C32 C33 1.472(7) . ?
C33 C34 1.383(5) . ?
C34 C35 1.394(6) . ?
C35 C36 1.396(4) . ?
C35 C38 1.515(4) . ?
C36 C37 1.393(7) . ?
C38 N42 1.452(5) . ?
N41 C45 1.349(3) . ?
N41 N42 1.349(3) . ?
N42 C43 1.360(4) . ?
C43 C44 1.356(5) . ?
C44 C45 1.414(4) . ?
C45 C52 1.459(4) . ?
N51 C52 1.345(3) . ?
N51 C52 1.345(3) 3_575 ?
C52 C53 1.395(4) . ?
C53 C54 1.395(4) . ?
C54 C53 1.395(4) 3_575 ?
