Reactions of triosmium and triruthenium clusters with 2-ethynylpyridine: new modes for alkyne C‒C bond coupling and C‒H bond activation
Joy, Md. Tuhinur R.; Roknuzzaman,; Hossain, Md. Emdad; Ghosh, Shishir; Tocher, Derek A.; Richmond, Michael G.; Kabir, Shariff E.; RSC Advances 10 (2020) 30671–30682; doi:10.1039/D0RA05393G

data_7241081
_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  t~exp~   \w     \q     \k     \f   Frames
  1  \w     13.00  72.00   1.00    1.70    --   11.17  38.00   0.00   59
  2  \w     -3.00  87.00   1.00    1.70    --   11.17  77.00   0.00   90
  3  \w     -9.00  83.00   1.00    1.70    --   11.17  57.00 -90.00   92
  4  \w     -8.00  57.00   1.00    1.70    --   11.17-107.00  91.00   65
  5  \w    -20.00  52.00   1.00    1.70    --   11.17 -99.00 -30.00   72
  6  \w    -17.00  54.00   1.00    1.70    --   11.17-102.00-144.96   71
  7  \w    -84.00 -39.00   1.00    1.70    --  -10.07 -38.00 150.00   45
  8  \w    -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       '\w 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+0.001xFc^2^\l^3^/sin(2\q)]^-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/[\s^2^(Fo^2^)+(0.0306P)^2^] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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
_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