#------------------------------------------------------------------------------
#$Date: 2020-10-06 14:14:12 +0300 (Tue, 06 Oct 2020) $
#$Revision: 257975 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/10/7241081.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_7241081
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         'C17 H6 N O10 Os3'
_chemical_formula_sum            'C17 H6 N O10 Os3'
_chemical_formula_weight         954.83
_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     iterative
_audit_creation_date             2018-01-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2020-06-13 deposited with the CCDC.	2020-08-19 downloaded from the CCDC.
;
_cell_angle_alpha                100.068(4)
_cell_angle_beta                 92.632(4)
_cell_angle_gamma                111.204(4)
_cell_formula_units_Z            2
_cell_length_a                   8.7108(4)
_cell_length_b                   9.1324(4)
_cell_length_c                   14.1005(6)
_cell_measurement_reflns_used    9337
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      29.1180
_cell_measurement_theta_min      4.0880
_cell_volume                     1022.35(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2031
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     13.00  72.00   1.00    1.70    --   11.17  38.00   0.00   59
  2  ω     -3.00  87.00   1.00    1.70    --   11.17  77.00   0.00   90
  3  ω     -9.00  83.00   1.00    1.70    --   11.17  57.00 -90.00   92
  4  ω     -8.00  57.00   1.00    1.70    --   11.17-107.00  91.00   65
  5  ω    -20.00  52.00   1.00    1.70    --   11.17 -99.00 -30.00   72
  6  ω    -17.00  54.00   1.00    1.70    --   11.17-102.00-144.96   71
  7  ω    -84.00 -39.00   1.00    1.70    --  -10.07 -38.00 150.00   45
  8  ω    -13.00  85.00   1.00    1.70    --   11.17  38.00 150.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0128328000
_diffrn_orient_matrix_UB_12      -0.0659363000
_diffrn_orient_matrix_UB_13      -0.0386527000
_diffrn_orient_matrix_UB_21      -0.0304152000
_diffrn_orient_matrix_UB_22      -0.0536837000
_diffrn_orient_matrix_UB_23      0.0316495000
_diffrn_orient_matrix_UB_31      -0.0815355000
_diffrn_orient_matrix_UB_32      -0.0041184000
_diffrn_orient_matrix_UB_33      -0.0123239000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0553
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15181
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         3.427
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    18.652
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.13668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.102
_exptl_crystal_description       block
_exptl_crystal_F_000             846
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.258
_refine_diff_density_min         -1.455
_refine_diff_density_rms         0.249
_refine_ls_extinction_coef       0.00091(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         4006
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0269
_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)+(0.0306P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0623
_refine_ls_wR_factor_ref         0.0641
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3714
_reflns_number_total             4006
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0ra05393g2.cif
_cod_data_source_block           xstr0803
_cod_depositor_comments
'Adding full bibliography for 7241081--7241085.cif.'
_cod_original_cell_volume        1022.35(8)
_cod_database_code               7241081
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'Os3 C17 N1 O10 H7'
_chemical_oxdiff_usercomment     TR-06A
_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.
;
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C11(H11), C12(H12)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C17(H17)
;
_olex2_date_sample_data_collection 2018-01-19
_olex2_exptl_crystal_mounting_method 'Nylon Loop'
_olex2_submission_original_sample_id xstr0803
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.462
_oxdiff_exptl_absorpt_empirical_full_min 0.488
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
Os1 Os 0.17218(3) 0.63366(3) 0.81565(2) 0.01219(9) Uani 1 1 d . . . . .
Os2 Os 0.39717(3) 0.80451(3) 0.69870(2) 0.01143(9) Uani 1 1 d . . . . .
Os3 Os 0.70876(3) 0.98668(3) 0.63617(2) 0.01276(9) Uani 1 1 d . . . . .
O1 O -0.0992(6) 0.6264(6) 0.6695(4) 0.0286(12) Uani 1 1 d . . . . .
O2 O 0.1270(6) 0.9020(6) 0.9648(4) 0.0286(12) Uani 1 1 d . . . . .
O3 O -0.0531(6) 0.3484(6) 0.8909(4) 0.0309(12) Uani 1 1 d . . . . .
O4 O 0.2284(6) 1.0381(6) 0.6791(4) 0.0359(13) Uani 1 1 d . . . . .
O5 O 0.2818(6) 0.6554(6) 0.4823(3) 0.0277(11) Uani 1 1 d . . . . .
O6 O 0.5775(5) 1.0073(5) 0.8984(3) 0.0225(10) Uani 1 1 d . . . . .
O7 O 0.6342(6) 1.2787(6) 0.7348(4) 0.0312(12) Uani 1 1 d . . . . .
O8 O 0.9218(6) 0.9674(7) 0.8129(4) 0.0336(13) Uani 1 1 d . . . . .
O9 O 0.6557(6) 0.6570(6) 0.5090(4) 0.0267(11) Uani 1 1 d . . . . .
O10 O 0.9971(6) 1.1794(6) 0.5399(4) 0.0342(13) Uani 1 1 d . . . . .
N1 N 0.3940(6) 0.6463(6) 0.8951(4) 0.0126(11) Uani 1 1 d . . . . .
C1 C 0.0013(8) 0.6279(8) 0.7247(5) 0.0204(15) Uani 1 1 d . . . . .
C2 C 0.1410(7) 0.8026(8) 0.9113(5) 0.0165(14) Uani 1 1 d . . . . .
C3 C 0.0338(8) 0.4572(9) 0.8649(5) 0.0203(15) Uani 1 1 d . . . . .
C4 C 0.2942(8) 0.9513(8) 0.6855(5) 0.0187(14) Uani 1 1 d . . . . .
C5 C 0.3238(8) 0.7076(8) 0.5620(5) 0.0185(14) Uani 1 1 d . . . . .
C6 C 0.5079(8) 0.9301(7) 0.8261(5) 0.0161(14) Uani 1 1 d . . . . .
C7 C 0.6651(7) 1.1745(8) 0.7004(5) 0.0191(14) Uani 1 1 d . . . . .
C8 C 0.8428(8) 0.9737(8) 0.7493(5) 0.0199(15) Uani 1 1 d . . . . .
C9 C 0.6791(8) 0.7761(8) 0.5583(5) 0.0198(14) Uani 1 1 d . . . . .
C10 C 0.8917(8) 1.1066(8) 0.5761(5) 0.0242(16) Uani 1 1 d . . . . .
C11 C 0.2863(8) 0.5475(7) 0.7081(5) 0.0180(14) Uani 1 1 d . . . . .
H11 H 0.2241 0.4626 0.6521 0.022 Uiso 1 1 calc R . . . .
C12 C 0.4604(7) 0.5903(7) 0.7354(4) 0.0151(13) Uani 1 1 d . . . . .
H12 H 0.5228 0.5437 0.6918 0.018 Uiso 1 1 calc R . . . .
C13 C 0.5109(7) 0.6291(7) 0.8393(5) 0.0161(13) Uani 1 1 d . . . . .
C14 C 0.6673(7) 0.6519(8) 0.8831(5) 0.0200(15) Uani 1 1 d . . . . .
H14 H 0.7479 0.6396 0.8450 0.024 Uiso 1 1 calc R . . . .
C15 C 0.7014(8) 0.6921(8) 0.9811(5) 0.0224(15) Uani 1 1 d . . . . .
H15 H 0.8063 0.7093 1.0099 0.027 Uiso 1 1 calc R . . . .
C16 C 0.5816(8) 0.7079(8) 1.0386(5) 0.0210(15) Uani 1 1 d . . . . .
H16 H 0.6036 0.7346 1.1058 0.025 Uiso 1 1 calc R . . . .
C17 C 0.4291(8) 0.6827(7) 0.9927(5) 0.0178(14) Uani 1 1 d . . . . .
H17 H 0.3465 0.6911 1.0303 0.021 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'
Os Os -1.2165 7.6030 '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
N1 Os1 Os2 83.17(13) . . ?
C1 Os1 Os2 86.5(2) . . ?
C1 Os1 N1 168.7(2) . . ?
C1 Os1 C2 92.2(3) . . ?
C1 Os1 C3 94.5(3) . . ?
C1 Os1 C11 92.0(3) . . ?
C2 Os1 Os2 104.10(19) . . ?
C2 Os1 N1 94.6(2) . . ?
C2 Os1 C11 154.7(3) . . ?
C3 Os1 Os2 159.21(19) . . ?
C3 Os1 N1 93.6(2) . . ?
C3 Os1 C2 96.6(3) . . ?
C3 Os1 C11 107.9(3) . . ?
C11 Os1 Os2 51.31(17) . . ?
C11 Os1 N1 78.1(2) . . ?
Os1 Os2 Os3 159.593(12) . . ?
C4 Os2 Os1 96.3(2) . . ?
C4 Os2 Os3 96.0(2) . . ?
C4 Os2 C5 88.3(3) . . ?
C4 Os2 C6 90.9(3) . . ?
C4 Os2 C11 130.1(3) . . ?
C4 Os2 C12 164.3(2) . . ?
C5 Os2 Os1 110.54(18) . . ?
C5 Os2 Os3 86.08(18) . . ?
C5 Os2 C6 168.7(3) . . ?
C5 Os2 C11 80.2(3) . . ?
C5 Os2 C12 95.1(2) . . ?
C6 Os2 Os1 80.71(18) . . ?
C6 Os2 Os3 82.81(18) . . ?
C6 Os2 C11 108.6(2) . . ?
C6 Os2 C12 88.6(2) . . ?
C11 Os2 Os1 45.98(15) . . ?
C11 Os2 Os3 130.92(16) . . ?
C11 Os2 C12 36.5(2) . . ?
C12 Os2 Os1 68.21(14) . . ?
C12 Os2 Os3 99.51(15) . . ?
C7 Os3 Os2 84.35(18) . . ?
C7 Os3 C8 96.2(3) . . ?
C8 Os3 Os2 93.45(18) . . ?
C9 Os3 Os2 82.52(18) . . ?
C9 Os3 C7 162.3(3) . . ?
C9 Os3 C8 96.4(3) . . ?
C10 Os3 Os2 170.3(2) . . ?
C10 Os3 C7 95.1(3) . . ?
C10 Os3 C8 96.2(3) . . ?
C10 Os3 C9 95.8(3) . . ?
C13 N1 Os1 114.4(4) . . ?
C17 N1 Os1 125.8(4) . . ?
C17 N1 C13 119.5(5) . . ?
O1 C1 Os1 178.8(6) . . ?
O2 C2 Os1 177.9(6) . . ?
O3 C3 Os1 177.2(6) . . ?
O4 C4 Os2 178.0(6) . . ?
O5 C5 Os2 178.1(6) . . ?
O6 C6 Os2 177.1(5) . . ?
O7 C7 Os3 177.2(6) . . ?
O8 C8 Os3 178.7(6) . . ?
O9 C9 Os3 175.4(6) . . ?
O10 C10 Os3 178.1(7) . . ?
Os1 C11 Os2 82.7(2) . . ?
C12 C11 Os1 113.1(4) . . ?
C12 C11 Os2 76.4(4) . . ?
C11 C12 Os2 67.1(3) . . ?
C11 C12 C13 114.9(5) . . ?
C13 C12 Os2 106.5(4) . . ?
N1 C13 C12 115.0(5) . . ?
N1 C13 C14 119.6(6) . . ?
C14 C13 C12 125.4(5) . . ?
C15 C14 C13 120.0(6) . . ?
C14 C15 C16 120.6(6) . . ?
C17 C16 C15 117.6(6) . . ?
N1 C17 C16 122.7(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
Os1 Os2 2.8248(4) . ?
Os1 N1 2.144(5) . ?
Os1 C1 1.899(7) . ?
Os1 C2 1.971(7) . ?
Os1 C3 1.896(7) . ?
Os1 C11 2.048(6) . ?
Os2 Os3 2.8945(4) . ?
Os2 C4 1.891(7) . ?
Os2 C5 1.946(7) . ?
Os2 C6 1.948(7) . ?
Os2 C11 2.223(6) . ?
Os2 C12 2.346(6) . ?
Os3 C7 1.966(7) . ?
Os3 C8 1.979(7) . ?
Os3 C9 1.961(7) . ?
Os3 C10 1.908(7) . ?
O1 C1 1.140(8) . ?
O2 C2 1.121(7) . ?
O3 C3 1.142(8) . ?
O4 C4 1.146(8) . ?
O5 C5 1.128(8) . ?
O6 C6 1.134(8) . ?
O7 C7 1.118(8) . ?
O8 C8 1.127(8) . ?
O9 C9 1.127(8) . ?
O10 C10 1.125(8) . ?
N1 C13 1.352(8) . ?
N1 C17 1.351(8) . ?
C11 C12 1.437(9) . ?
C12 C13 1.453(9) . ?
C13 C14 1.397(9) . ?
C14 C15 1.356(9) . ?
C15 C16 1.383(9) . ?
C16 C17 1.373(9) . ?
