#------------------------------------------------------------------------------
#$Date: 2020-06-05 13:59:00 +0300 (Fri, 05 Jun 2020) $
#$Revision: 252828 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/43/7704318.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_7704318
loop_
_publ_author_name
'Kang, Shi-Rui'
'Zhou, Zi-Qin'
'Xiong, Chang-Feng'
'Liu, Bin'
'McGrady, John E.'
'Obies, Mohammed'
'Liu, Chao'
'He, Piao'
'Yi, Xiao-Yi'
_publ_section_title
;
 Structural, spectroscopic and electronic properties of a family of
 face-shared bi-octahedral Ru₂<sup>5+/6+</sup> complexes with a
 bridging 2,5-di(2-pyridyl)pyrrolide ligand.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7053
_journal_page_last               7059
_journal_paper_doi               10.1039/d0dt01325k
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C14 H10 N3 Ru0.333'
_chemical_formula_sum            'C14 H10 N3 Ru0.33'
_chemical_formula_weight         253.94
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-03-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-03-22 deposited with the CCDC.	2020-05-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   18.0733(8)
_cell_length_b                   18.0733(8)
_cell_length_c                   18.3272(13)
_cell_measurement_reflns_used    4520
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.11
_cell_measurement_theta_min      1.89
_cell_volume                     5184.4(5)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/2 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            28139
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.531
_diffrn_reflns_theta_min         1.711
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.500
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6925
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_description       block
_exptl_crystal_F_000             2334
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.415
_refine_diff_density_min         -0.821
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         3194
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0394
_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)+(0.0640P)²+6.7879P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1141
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2635
_reflns_number_total             3194
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt01325k2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7704316--7704319.cif.'
_cod_original_cell_volume        5184.4(6)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7704318
_shelxl_version_number           2013-2
_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_max   0.907
_shelx_estimated_absorpt_t_min   0.907
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Sof(Ru)=0.33333*(1-FVAR(2))
 Sof(Ru01)=0.33333*FVAR(2)
3.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C4A(H4A), C11B(H11B), C8C(H8C), C12D(H12D), C13E(H13E), C7F(H7F),
 C3G(H3G), C1H(H1H), C2I(H2I)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru01 Ru 0.6667 0.3333 0.54533(2) 0.02722(12) Uani 0.9026(14) 3 d S T P A 1
N2 N 0.58866(12) 0.37610(12) 0.59730(10) 0.0333(4) Uani 1 1 d . . . . .
N3 N 0.69862(12) 0.44198(12) 0.48590(11) 0.0362(4) Uani 1 1 d . . . . .
N1 N 0.54582(13) 0.25546(13) 0.71850(11) 0.0407(5) Uani 1 1 d . . . . .
C6 C 0.52043(15) 0.34965(15) 0.64367(13) 0.0370(5) Uani 1 1 d . . . . .
C5 C 0.48995(15) 0.27851(15) 0.69435(13) 0.0374(5) Uani 1 1 d . . . . .
C9 C 0.59722(16) 0.44783(15) 0.56288(13) 0.0386(5) Uani 1 1 d . . . . .
C10 C 0.65862(15) 0.48572(15) 0.50518(13) 0.0376(5) Uani 1 1 d . . . . .
C14 C 0.75558(17) 0.47312(17) 0.43057(15) 0.0471(6) Uani 1 1 d . . . . .
H14 H 0.7837 0.4438 0.4176 0.057 Uiso 1 1 calc R U . . .
C4A C 0.40532(17) 0.23696(18) 0.71910(16) 0.0485(6) Uani 1 1 d . . . . .
H4A H 0.3680 0.2553 0.7040 0.058 Uiso 1 1 calc R U . . .
C11B C 0.67558(19) 0.56071(16) 0.46825(16) 0.0493(6) Uani 1 1 d . . . . .
H11B H 0.6477 0.5900 0.4819 0.059 Uiso 1 1 calc R U . . .
C8C C 0.5360(2) 0.46713(19) 0.58773(16) 0.0544(7) Uani 1 1 d . . . . .
H8C H 0.5292 0.5127 0.5731 0.065 Uiso 1 1 calc R U . . .
C12D C 0.7333(2) 0.59053(17) 0.41204(17) 0.0566(7) Uani 1 1 d . . . . .
H12D H 0.7450 0.6402 0.3873 0.068 Uiso 1 1 calc R U . . .
C13E C 0.77409(19) 0.54566(18) 0.39250(17) 0.0549(7) Uani 1 1 d . . . . .
H13E H 0.8132 0.5644 0.3543 0.066 Uiso 1 1 calc R U . . .
C7F C 0.48728(19) 0.4051(2) 0.63858(17) 0.0529(7) Uani 1 1 d . . . . .
H7F H 0.4411 0.4010 0.6646 0.063 Uiso 1 1 calc R U . . .
C3G C 0.37776(19) 0.1686(2) 0.76609(16) 0.0564(7) Uani 1 1 d . . . . .
H3G H 0.3216 0.1400 0.7826 0.068 Uiso 1 1 calc R U . . .
C1H C 0.51738(19) 0.18826(17) 0.76352(15) 0.0494(6) Uani 1 1 d . . . . .
H1H H 0.5556 0.1712 0.7789 0.059 Uiso 1 1 calc R U . . .
C2I C 0.4341(2) 0.14311(18) 0.78821(16) 0.0567(7) Uani 1 1 d . . . . .
H2I H 0.4166 0.0965 0.8192 0.068 Uiso 1 1 calc R U . . .
Ru Ru 0.6667 0.3333 0.6659(4) 0.079(2) Uani 0.0974(14) 3 d S T P A 2
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'
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
N2 Ru01 N2 101.71(6) 3_665 . ?
N2 Ru01 N2 101.71(6) 2_655 3_665 ?
N2 Ru01 N2 101.71(6) 2_655 . ?
N3 Ru01 N2 79.19(7) 3_665 3_665 ?
N3 Ru01 N2 84.26(7) 2_655 . ?
N3 Ru01 N2 79.18(7) 2_655 2_655 ?
N3 Ru01 N2 79.19(7) . . ?
N3 Ru01 N2 173.57(7) . 2_655 ?
N3 Ru01 N2 84.25(7) 3_665 2_655 ?
N3 Ru01 N2 173.57(7) 2_655 3_665 ?
N3 Ru01 N2 84.26(7) . 3_665 ?
N3 Ru01 N2 173.57(7) 3_665 . ?
N3 Ru01 N3 94.62(7) 2_655 . ?
N3 Ru01 N3 94.62(8) 3_665 . ?
N3 Ru01 N3 94.62(8) 3_665 2_655 ?
C6 N2 Ru01 142.13(16) . . ?
C6 N2 C9 105.65(19) . . ?
C6 N2 Ru 98.1(2) . . ?
C9 N2 Ru01 110.57(15) . . ?
C9 N2 Ru 140.27(16) . . ?
C10 N3 Ru01 116.13(15) . . ?
C14 N3 Ru01 125.88(17) . . ?
C14 N3 C10 118.0(2) . . ?
C5 N1 Ru 108.93(19) . . ?
C1H N1 C5 118.4(2) . . ?
C1H N1 Ru 132.4(2) . . ?
N2 C6 C5 125.5(2) . . ?
N2 C6 C7F 109.9(2) . . ?
C7F C6 C5 124.5(2) . . ?
N1 C5 C6 118.2(2) . . ?
N1 C5 C4A 121.0(2) . . ?
C4A C5 C6 120.7(2) . . ?
N2 C9 C10 118.8(2) . . ?
N2 C9 C8C 110.9(2) . . ?
C8C C9 C10 130.0(2) . . ?
N3 C10 C9 115.1(2) . . ?
N3 C10 C11B 120.9(2) . . ?
C11B C10 C9 124.0(2) . . ?
N3 C14 H14 118.3 . . ?
N3 C14 C13E 123.4(3) . . ?
C13E C14 H14 118.3 . . ?
C5 C4A H4A 120.3 . . ?
C3G C4A C5 119.4(3) . . ?
C3G C4A H4A 120.3 . . ?
C10 C11B H11B 120.1 . . ?
C12D C11B C10 119.8(3) . . ?
C12D C11B H11B 120.1 . . ?
C9 C8C H8C 126.8 . . ?
C7F C8C C9 106.3(2) . . ?
C7F C8C H8C 126.8 . . ?
C11B C12D H12D 120.4 . . ?
C11B C12D C13E 119.1(3) . . ?
C13E C12D H12D 120.4 . . ?
C14 C13E C12D 118.7(3) . . ?
C14 C13E H13E 120.6 . . ?
C12D C13E H13E 120.6 . . ?
C6 C7F H7F 126.4 . . ?
C8C C7F C6 107.3(2) . . ?
C8C C7F H7F 126.4 . . ?
C4A C3G H3G 120.3 . . ?
C2I C3G C4A 119.3(3) . . ?
C2I C3G H3G 120.3 . . ?
N1 C1H H1H 118.4 . . ?
N1 C1H C2I 123.2(3) . . ?
C2I C1H H1H 118.4 . . ?
C3G C2I C1H 118.5(3) . . ?
C3G C2I H2I 120.7 . . ?
C1H C2I H2I 120.7 . . ?
N2 Ru N2 92.8(2) 2_655 3_665 ?
N2 Ru N2 92.8(2) 2_655 . ?
N2 Ru N2 92.8(2) 3_665 . ?
N1 Ru N2 82.63(8) 2_655 2_655 ?
N1 Ru N2 173.5(4) 2_655 . ?
N1 Ru N2 82.63(8) . . ?
N1 Ru N2 82.63(8) 3_665 3_665 ?
N1 Ru N2 82.75(8) 3_665 . ?
N1 Ru N2 173.5(4) . 3_665 ?
N1 Ru N2 173.5(4) 3_665 2_655 ?
N1 Ru N2 82.76(8) 2_655 3_665 ?
N1 Ru N2 82.75(8) . 2_655 ?
N1 Ru N1 101.4(2) 2_655 3_665 ?
N1 Ru N1 101.4(2) 3_665 . ?
N1 Ru N1 101.4(2) 2_655 . ?
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
Ru01 N2 2.1406(19) 2_655 ?
Ru01 N2 2.1406(19) . ?
Ru01 N2 2.1406(19) 3_665 ?
Ru01 N3 2.0596(19) 3_665 ?
Ru01 N3 2.0595(19) . ?
Ru01 N3 2.0595(19) 2_655 ?
N2 C6 1.372(3) . ?
N2 C9 1.379(3) . ?
N2 Ru 2.292(5) . ?
N3 C10 1.358(3) . ?
N3 C14 1.351(3) . ?
N1 C5 1.345(3) . ?
N1 C1H 1.340(3) . ?
N1 Ru 2.147(4) . ?
C6 C5 1.453(3) . ?
C6 C7F 1.405(3) . ?
C5 C4A 1.400(3) . ?
C9 C10 1.435(3) . ?
C9 C8C 1.392(4) . ?
C10 C11B 1.405(3) . ?
C14 H14 0.9300 . ?
C14 C13E 1.371(4) . ?
C4A H4A 0.9300 . ?
C4A C3G 1.379(4) . ?
C11B H11B 0.9300 . ?
C11B C12D 1.370(4) . ?
C8C H8C 0.9300 . ?
C8C C7F 1.383(4) . ?
C12D H12D 0.9300 . ?
C12D C13E 1.388(4) . ?
C13E H13E 0.9300 . ?
C7F H7F 0.9300 . ?
C3G H3G 0.9300 . ?
C3G C2I 1.371(5) . ?
C1H H1H 0.9300 . ?
C1H C2I 1.382(4) . ?
C2I H2I 0.9300 . ?
Ru N2 2.292(5) 2_655 ?
Ru N2 2.292(5) 3_665 ?
Ru N1 2.146(4) 2_655 ?
Ru N1 2.146(4) 3_665 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ru01 N2 C6 C5 20.7(4) . . . . ?
Ru01 N2 C6 C7F -163.2(2) . . . . ?
Ru01 N2 C9 C10 -5.2(3) . . . . ?
Ru01 N2 C9 C8C 169.46(19) . . . . ?
Ru01 N3 C10 C9 -2.1(3) . . . . ?
Ru01 N3 C10 C11B -179.96(19) . . . . ?
Ru01 N3 C14 C13E 179.6(2) . . . . ?
N2 C6 C5 N1 25.6(3) . . . . ?
N2 C6 C5 C4A -156.4(2) . . . . ?
N2 C6 C7F C8C 0.2(3) . . . . ?
N2 C9 C10 N3 5.0(3) . . . . ?
N2 C9 C10 C11B -177.2(2) . . . . ?
N2 C9 C8C C7F -0.6(3) . . . . ?
N3 C10 C11B C12D -0.1(4) . . . . ?
N3 C14 C13E C12D 0.9(5) . . . . ?
N1 C5 C4A C3G -3.3(4) . . . . ?
N1 C1H C2I C3G -0.5(4) . . . . ?
C6 N2 C9 C10 -173.9(2) . . . . ?
C6 N2 C9 C8C 0.7(3) . . . . ?
C6 C5 C4A C3G 178.8(2) . . . . ?
C5 N1 C1H C2I -2.1(4) . . . . ?
C5 C6 C7F C8C 176.4(2) . . . . ?
C5 C4A C3G C2I 0.6(4) . . . . ?
C9 N2 C6 C5 -176.7(2) . . . . ?
C9 N2 C6 C7F -0.6(3) . . . . ?
C9 C10 C11B C12D -177.7(3) . . . . ?
C9 C8C C7F C6 0.3(4) . . . . ?
C10 N3 C14 C13E -0.9(4) . . . . ?
C10 C9 C8C C7F 173.2(3) . . . . ?
C10 C11B C12D C13E 0.1(5) . . . . ?
C14 N3 C10 C9 178.3(2) . . . . ?
C14 N3 C10 C11B 0.5(4) . . . . ?
C4A C3G C2I C1H 1.2(4) . . . . ?
C11B C12D C13E C14 -0.5(5) . . . . ?
C8C C9 C10 N3 -168.4(3) . . . . ?
C8C C9 C10 C11B 9.4(5) . . . . ?
C7F C6 C5 N1 -150.0(3) . . . . ?
C7F C6 C5 C4A 28.0(4) . . . . ?
C1H N1 C5 C6 -178.0(2) . . . . ?
C1H N1 C5 C4A 4.0(4) . . . . ?
Ru N2 C6 C5 -28.9(3) . . . . ?
Ru N2 C6 C7F 147.2(2) . . . . ?
Ru N2 C9 C10 61.7(4) . . . . ?
Ru N2 C9 C8C -123.6(4) . . . . ?
Ru N1 C5 C6 -3.0(3) . . . . ?
Ru N1 C5 C4A 179.1(3) . . . . ?
Ru N1 C1H C2I -175.8(3) . . . . ?
