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_7241085
_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         'C16 H6 N O9 Os3'
_chemical_formula_sum            'C16 H6 N O9 Os3'
_chemical_formula_weight         926.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-07-02
_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                90
_cell_angle_beta                 91.697(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.1249(2)
_cell_length_b                   15.2910(4)
_cell_length_c                   15.3121(4)
_cell_measurement_reflns_used    16199
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      29.2840
_cell_measurement_theta_min      3.8680
_cell_volume                     1901.51(8)
_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    'ShelXS (Sheldrick, 2008)'
_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  85.00   1.00    2.42    --   11.17  38.00 -60.00   98
  2  \w    -14.00  84.00   1.00    2.42    --   11.17  57.00  30.00   98
  3  \w    -15.00  87.00   1.00    2.42    --   11.17  77.00 150.00  102
  4  \w    -19.00  52.00   1.00    2.42    --   11.17 -99.00   0.00   71
  5  \w     38.00  91.00   1.00    2.42    --   11.17-178.00 -90.00   53
  6  \w    -18.00  52.00   1.00    2.42    --   11.17 -99.00 120.00   70
  7  \w    -54.00  39.00   1.00    2.42    --   11.17 -57.00-120.00   93
  8  \w    -86.00 -61.00   1.00    2.42    --  -10.07 154.00  90.29   25
;
_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      -0.0475379000
_diffrn_orient_matrix_UB_12      0.0251358000
_diffrn_orient_matrix_UB_13      -0.0304272000
_diffrn_orient_matrix_UB_21      0.0154812000
_diffrn_orient_matrix_UB_22      0.0380884000
_diffrn_orient_matrix_UB_23      0.0253769000
_diffrn_orient_matrix_UB_31      0.0716159000
_diffrn_orient_matrix_UB_32      0.0084616000
_diffrn_orient_matrix_UB_33      -0.0239872000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0623
_diffrn_reflns_av_unetI/netI     0.0327
_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       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30729
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_min         3.168
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    20.047
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41160
_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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    3.237
_exptl_crystal_description       block
_exptl_crystal_F_000             1636
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.062
_refine_diff_density_min         -1.497
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         4142
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0211
_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^)+(0.0168P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0459
_refine_ls_wR_factor_ref         0.0471
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3857
_reflns_number_total             4142
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra05393g2.cif
_cod_data_source_block           xstr0818
_cod_depositor_comments
'Adding full bibliography for 7241081--7241085.cif.'
_cod_original_cell_volume        1901.52(8)
_cod_database_code               7241085
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'Os3 O9 N1 C16 H7'
_chemical_oxdiff_usercomment     PM-8A
_reflns_odcompleteness_completeness 99.70
_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 Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13)
;
_olex2_date_sample_data_collection 2018-02-08
_olex2_exptl_crystal_mounting_method 'Nylon Loop'
_olex2_submission_original_sample_id xstr0818
_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 2.084
_oxdiff_exptl_absorpt_empirical_full_min 0.701