#------------------------------------------------------------------------------
#$Date: 2020-10-06 14:14:12 +0300 (Tue, 06 Oct 2020) $
#$Revision: 257975 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/10/7241083.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_7241083
loop_
_publ_author_name
'Joy, Md. Tuhinur R.'
Roknuzzaman,
'Hossain, Md. Emdad'
'Ghosh, Shishir'
'Tocher, Derek A.'
'Richmond, Michael G.'
'Kabir, Shariff E.'
_publ_section_title
;
 Reactions of triosmium and triruthenium clusters with 2-ethynylpyridine:
 new modes for alkyne C--C bond coupling and C--H bond activation
;
_journal_issue                   51
_journal_name_full               'RSC Advances'
_journal_page_first              30671
_journal_page_last               30682
_journal_paper_doi               10.1039/D0RA05393G
_journal_volume                  10
_journal_year                    2020
_chemical_formula_moiety         'C22 H10 N2 O8 Ru3'
_chemical_formula_sum            'C22 H10 N2 O8 Ru3'
_chemical_formula_weight         733.53
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-07-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-13 deposited with the CCDC.	2020-08-19 downloaded from the CCDC.
;
_cell_angle_alpha                97.65(3)
_cell_angle_beta                 94.716(17)
_cell_angle_gamma                106.30(2)
_cell_formula_units_Z            2
_cell_length_a                   8.187(5)
_cell_length_b                   9.641(6)
_cell_length_c                   15.139(9)
_cell_measurement_reflns_used    9879
_cell_measurement_temperature    193(1)
_cell_measurement_theta_max      27.094
_cell_measurement_theta_min      2.228
_cell_volume                     1127.7(12)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      193(1)
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-III CCD diffractometer'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32047
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.155
_diffrn_reflns_theta_min         2.231
_exptl_absorpt_coefficient_mu    2.036
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6583
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0706 before and 0.0544 after correction. The Ratio of minimum to maximum transmission is 0.8830. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.160
_exptl_crystal_description       plate
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.116
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.031
_refine_diff_density_max         1.239
_refine_diff_density_min         -0.827
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5010
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0323
_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)+(0.0491P)²+0.7111P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0854
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4049
_reflns_number_total             5010
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0ra05393g2.cif
_cod_data_source_block           tr_63b_0m
_cod_depositor_comments
'Adding full bibliography for 7241081--7241085.cif.'
_cod_database_code               7241083
_shelx_shelxl_version_number     2018/3
_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   0.940
_shelx_estimated_absorpt_t_min   0.798
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C10(H10), C12(H12)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
Ru1 Ru 0.77708(4) 0.74776(3) 0.84665(2) 0.02231(10) Uani 1 1 d . . . . .
O1 O 0.5521(5) 0.9392(4) 0.8989(3) 0.0543(10) Uani 1 1 d . . . . .
N1 N 0.5921(4) 0.3791(3) 0.8066(2) 0.0243(7) Uani 1 1 d . . . . .
C1 C 0.6385(6) 0.8693(5) 0.8821(3) 0.0348(10) Uani 1 1 d . . . . .
Ru2 Ru 0.84632(4) 0.62744(3) 0.68125(2) 0.02047(9) Uani 1 1 d . . . . .
O2 O 1.1275(4) 0.9514(4) 0.9345(2) 0.0425(8) Uani 1 1 d . . . . .
N2 N 0.5645(5) 0.7635(4) 0.5057(2) 0.0351(9) Uani 1 1 d . . . . .
C2 C 0.9958(6) 0.8759(5) 0.9061(3) 0.0293(9) Uani 1 1 d . . . . .
Ru3 Ru 0.86453(4) 0.48113(3) 0.83366(2) 0.02308(10) Uani 1 1 d . . . . .
O3 O 0.6856(5) 0.5978(4) 1.0108(2) 0.0457(9) Uani 1 1 d . . . . .
C3 C 0.7252(5) 0.6420(4) 0.9482(3) 0.0277(9) Uani 1 1 d . . . . .
C4 C 0.8255(5) 0.5484(5) 0.5577(3) 0.0310(10) Uani 1 1 d . . . . .
O4 O 0.8135(4) 0.5026(4) 0.4840(2) 0.0490(9) Uani 1 1 d . . . . .
O5 O 1.2297(4) 0.7646(4) 0.6951(2) 0.0488(9) Uani 1 1 d . . . . .
C5 C 1.0865(6) 0.7106(4) 0.6891(3) 0.0289(9) Uani 1 1 d . . . . .
C6 C 1.0988(6) 0.5813(5) 0.8675(3) 0.0291(9) Uani 1 1 d . . . . .
O6 O 1.2390(4) 0.6417(4) 0.8887(2) 0.0440(8) Uani 1 1 d . . . . .
C7 C 0.9008(5) 0.3203(5) 0.8789(3) 0.0331(10) Uani 1 1 d . . . . .
O7 O 0.9280(4) 0.2213(4) 0.9032(3) 0.0506(9) Uani 1 1 d . . . . .
C8 C 0.8904(5) 0.4270(4) 0.7059(3) 0.0226(8) Uani 1 1 d . . . . .
O8 O 0.9196(4) 0.3314(3) 0.6609(2) 0.0327(7) Uani 1 1 d . . . . .
C9 C 0.6013(5) 0.5968(4) 0.7475(3) 0.0229(8) Uani 1 1 d . . . . .
C10 C 0.5769(5) 0.6411(4) 0.6649(3) 0.0222(8) Uani 1 1 d . . . . .
H10 H 0.489273 0.580284 0.615364 0.027 Uiso 1 1 calc R . . . .
C11 C 0.6928(5) 0.7819(4) 0.6566(3) 0.0234(8) Uani 1 1 d . . . . .
C12 C 0.8124(5) 0.8442(4) 0.7330(3) 0.0244(8) Uani 1 1 d . . . . .
H12 H 0.904982 0.936392 0.734142 0.029 Uiso 1 1 calc R . . . .
C13 C 0.6811(5) 0.8452(4) 0.5727(3) 0.0246(8) Uani 1 1 d . . . . .
C14 C 0.7830(6) 0.9848(5) 0.5670(3) 0.0421(12) Uani 1 1 d . . . . .
H14 H 0.864637 1.040238 0.615370 0.050 Uiso 1 1 calc R . . . .
C15 C 0.7622(7) 1.0405(5) 0.4891(3) 0.0463(13) Uani 1 1 d . . . . .
H15 H 0.831516 1.133828 0.483010 0.056 Uiso 1 1 calc R . . . .
C16 C 0.6401(7) 0.9590(5) 0.4209(3) 0.0405(12) Uani 1 1 d . . . . .
H16 H 0.620778 0.995980 0.367891 0.049 Uiso 1 1 calc R . . . .
C17 C 0.5457(7) 0.8210(5) 0.4317(3) 0.0416(12) Uani 1 1 d . . . . .
H17 H 0.463230 0.764100 0.384088 0.050 Uiso 1 1 calc R . . . .
C18 C 0.5015(5) 0.4522(4) 0.7623(2) 0.0219(8) Uani 1 1 d . . . . .
C19 C 0.3270(5) 0.3924(4) 0.7372(3) 0.0275(9) Uani 1 1 d . . . . .
H19 H 0.265933 0.443483 0.705615 0.033 Uiso 1 1 calc R . . . .
C20 C 0.2426(5) 0.2594(5) 0.7582(3) 0.0326(10) Uani 1 1 d . . . . .
H20 H 0.123702 0.218639 0.741661 0.039 Uiso 1 1 calc R . . . .
C21 C 0.3359(6) 0.1861(5) 0.8041(3) 0.0352(10) Uani 1 1 d . . . . .
H21 H 0.281136 0.094607 0.819574 0.042 Uiso 1 1 calc R . . . .
C22 C 0.5077(6) 0.2481(4) 0.8267(3) 0.0302(9) Uani 1 1 d . . . . .
H22 H 0.570225 0.197233 0.857547 0.036 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'
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
C1 Ru1 Ru2 133.99(14) . . ?
C1 Ru1 C2 98.13(19) . . ?
C1 Ru1 Ru3 152.90(14) . . ?
C1 Ru1 C3 91.21(18) . . ?
C1 Ru1 C9 98.80(18) . . ?
C1 Ru1 C12 88.99(17) . . ?
Ru2 Ru1 Ru3 61.41(3) . . ?
C2 Ru1 Ru2 105.13(13) . . ?
C2 Ru1 Ru3 97.43(13) . . ?
C2 Ru1 C3 94.57(18) . . ?
C2 Ru1 C9 158.60(16) . . ?
C2 Ru1 C12 90.65(17) . . ?
C3 Ru1 Ru2 125.03(12) . . ?
C3 Ru1 Ru3 65.52(12) . . ?
C3 Ru1 C9 98.06(17) . . ?
C3 Ru1 C12 174.69(17) . . ?
C9 Ru1 Ru2 53.49(11) . . ?
C9 Ru1 Ru3 72.55(11) . . ?
C12 Ru1 Ru2 52.25(11) . . ?
C12 Ru1 Ru3 112.87(11) . . ?
C12 Ru1 C9 76.67(16) . . ?
C18 N1 Ru3 116.0(3) . . ?
C22 N1 Ru3 125.5(3) . . ?
C22 N1 C18 118.4(4) . . ?
O1 C1 Ru1 176.6(4) . . ?
Ru1 Ru2 Ru3 60.25(4) . . ?
C4 Ru2 Ru1 162.52(13) . . ?
C4 Ru2 Ru3 128.06(14) . . ?
C4 Ru2 C8 85.54(17) . . ?
C4 Ru2 C9 117.81(17) . . ?
C4 Ru2 C10 90.84(16) . . ?
C4 Ru2 C11 93.83(16) . . ?
C4 Ru2 C12 124.51(17) . . ?
C5 Ru2 Ru1 101.90(13) . . ?
C5 Ru2 Ru3 94.42(12) . . ?
C5 Ru2 C4 93.08(18) . . ?
C5 Ru2 C8 88.35(16) . . ?
C5 Ru2 C9 148.99(17) . . ?
C5 Ru2 C10 152.26(16) . . ?
C5 Ru2 C11 114.62(16) . . ?
C5 Ru2 C12 91.49(17) . . ?
C8 Ru2 Ru1 103.68(11) . . ?
C8 Ru2 Ru3 43.51(11) . . ?
C8 Ru2 C9 96.28(15) . . ?
C8 Ru2 C10 119.34(14) . . ?
C8 Ru2 C11 157.01(15) . . ?
C8 Ru2 C12 149.90(15) . . ?
C9 Ru2 Ru1 47.20(10) . . ?
C9 Ru2 Ru3 69.46(10) . . ?
C10 Ru2 Ru1 71.71(10) . . ?
C10 Ru2 Ru3 104.63(10) . . ?
C10 Ru2 C9 35.82(14) . . ?
C10 Ru2 C11 37.67(14) . . ?
C11 Ru2 Ru1 71.83(11) . . ?
C11 Ru2 Ru3 128.14(10) . . ?
C11 Ru2 C9 63.72(14) . . ?
C12 Ru2 Ru1 47.02(10) . . ?
C12 Ru2 Ru3 106.59(11) . . ?
C12 Ru2 C9 69.49(14) . . ?
C12 Ru2 C10 64.05(15) . . ?
C12 Ru2 C11 36.35(14) . . ?
C13 N2 C17 117.6(4) . . ?
O2 C2 Ru1 174.8(4) . . ?
Ru1 Ru3 Ru2 58.34(3) . . ?
N1 Ru3 Ru1 84.58(9) . . ?
N1 Ru3 Ru2 89.28(9) . . ?
C6 Ru3 Ru1 91.93(13) . . ?
C6 Ru3 N1 174.35(16) . . ?
C6 Ru3 Ru2 92.66(13) . . ?
C6 Ru3 C8 94.36(17) . . ?
C7 Ru3 Ru1 153.71(14) . . ?
C7 Ru3 N1 92.38(16) . . ?
C7 Ru3 Ru2 147.89(14) . . ?
C7 Ru3 C6 88.79(18) . . ?
C7 Ru3 C8 99.90(18) . . ?
C8 Ru3 Ru1 106.24(11) . . ?
C8 Ru3 N1 90.88(14) . . ?
C8 Ru3 Ru2 48.00(11) . . ?
O3 C3 Ru1 169.6(4) . . ?
O4 C4 Ru2 179.4(4) . . ?
O5 C5 Ru2 177.8(4) . . ?
O6 C6 Ru3 179.3(4) . . ?
O7 C7 Ru3 176.5(4) . . ?
Ru3 C8 Ru2 88.49(16) . . ?
O8 C8 Ru2 133.8(3) . . ?
O8 C8 Ru3 137.7(3) . . ?
Ru1 C9 Ru2 79.32(14) . . ?
C10 C9 Ru1 116.8(3) . . ?
C10 C9 Ru2 70.6(2) . . ?
C10 C9 C18 120.0(4) . . ?
C18 C9 Ru1 123.2(3) . . ?
C18 C9 Ru2 121.2(3) . . ?
Ru2 C10 H10 122.7 . . ?
C9 C10 Ru2 73.6(2) . . ?
C9 C10 H10 122.7 . . ?
C9 C10 C11 114.6(3) . . ?
C11 C10 Ru2 71.5(2) . . ?
C11 C10 H10 122.7 . . ?
C10 C11 Ru2 70.9(2) . . ?
C10 C11 C13 121.0(3) . . ?
C12 C11 Ru2 71.2(2) . . ?
C12 C11 C10 112.8(3) . . ?
C12 C11 C13 126.2(4) . . ?
C13 C11 Ru2 124.7(3) . . ?
Ru1 C12 Ru2 80.73(13) . . ?
Ru1 C12 H12 121.0 . . ?
Ru2 C12 H12 121.0 . . ?
C11 C12 Ru1 117.8(3) . . ?
C11 C12 Ru2 72.5(2) . . ?
C11 C12 H12 121.0 . . ?
N2 C13 C11 116.5(4) . . ?
N2 C13 C14 122.4(4) . . ?
C14 C13 C11 121.1(4) . . ?
C13 C14 H14 120.6 . . ?
C15 C14 C13 118.7(4) . . ?
C15 C14 H14 120.6 . . ?
C14 C15 H15 120.4 . . ?
C16 C15 C14 119.3(4) . . ?
C16 C15 H15 120.4 . . ?
C15 C16 H16 120.9 . . ?
C15 C16 C17 118.3(4) . . ?
C17 C16 H16 120.9 . . ?
N2 C17 C16 123.8(5) . . ?
N2 C17 H17 118.1 . . ?
C16 C17 H17 118.1 . . ?
N1 C18 C9 114.8(3) . . ?
N1 C18 C19 120.6(4) . . ?
C19 C18 C9 124.5(4) . . ?
C18 C19 H19 119.8 . . ?
C20 C19 C18 120.4(4) . . ?
C20 C19 H19 119.8 . . ?
C19 C20 H20 120.7 . . ?
C19 C20 C21 118.6(4) . . ?
C21 C20 H20 120.7 . . ?
C20 C21 H21 120.4 . . ?
C22 C21 C20 119.1(4) . . ?
C22 C21 H21 120.4 . . ?
N1 C22 C21 122.8(4) . . ?
N1 C22 H22 118.6 . . ?
C21 C22 H22 118.6 . . ?
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 C1 1.904(5) . ?
Ru1 Ru2 2.7868(15) . ?
Ru1 C2 1.933(5) . ?
Ru1 Ru3 2.8426(16) . ?
Ru1 C3 1.966(4) . ?
Ru1 C9 2.081(4) . ?
Ru1 C12 2.066(4) . ?
O1 C1 1.128(5) . ?
N1 Ru3 2.150(4) . ?
N1 C18 1.355(5) . ?
N1 C22 1.346(5) . ?
Ru2 Ru3 2.8747(15) . ?
Ru2 C4 1.898(5) . ?
Ru2 C5 1.891(5) . ?
Ru2 C8 2.137(4) . ?
Ru2 C9 2.279(4) . ?
Ru2 C10 2.241(4) . ?
Ru2 C11 2.250(4) . ?
Ru2 C12 2.233(4) . ?
O2 C2 1.130(5) . ?
N2 C13 1.329(5) . ?
N2 C17 1.330(6) . ?
Ru3 C6 1.882(5) . ?
Ru3 C7 1.863(5) . ?
Ru3 C8 1.980(4) . ?
O3 C3 1.124(5) . ?
C4 O4 1.131(5) . ?
O5 C5 1.131(5) . ?
C6 O6 1.128(5) . ?
C7 O7 1.138(5) . ?
C8 O8 1.163(5) . ?
C9 C10 1.391(5) . ?
C9 C18 1.461(5) . ?
C10 H10 0.9900 . ?
C10 C11 1.450(5) . ?
C11 C12 1.398(6) . ?
C11 C13 1.487(5) . ?
C12 H12 0.9900 . ?
C13 C14 1.389(6) . ?
C14 H14 0.9400 . ?
C14 C15 1.377(6) . ?
C15 H15 0.9400 . ?
C15 C16 1.362(7) . ?
C16 H16 0.9400 . ?
C16 C17 1.377(7) . ?
C17 H17 0.9400 . ?
C18 C19 1.381(6) . ?
C19 H19 0.9400 . ?
C19 C20 1.367(6) . ?
C20 H20 0.9400 . ?
C20 C21 1.383(6) . ?
C21 H21 0.9400 . ?
C21 C22 1.359(6) . ?
C22 H22 0.9400 . ?
