Alkyne activation and polyhedral reorganization in benzothiazolate-capped osmium clusters on reaction with diethyl acetylenedicarboxylate (DEAD) and ethyl propiolate
Mahid Uddin, Kh.; Chowdhury, Md. Arshad H.; Kamal Hossain, Md.; Ghosh, Shishir; Tocher, Derek A.; Richmond, Michael G.; Kabir, Shariff E.; Dalton Trans. 46 (2017) 13597–13609; doi:10.1039/C7DT02933K

data_1547174
_publ_section_title
;
 Alkyne activation and polyhedral reorganization in benzothiazolate-capped
 osmium clusters on reaction with diethyl acetylenedicarboxylate (DEAD)
 and ethyl propiolate
;
_journal_issue                   39
_journal_name_full               'Dalton Trans.'
_journal_page_first              13597
_journal_page_last               13609
_journal_paper_doi               10.1039/C7DT02933K
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C25 H17 N O13 Os3 S'
_chemical_formula_sum            'C25 H17 N O13 Os3 S'
_chemical_formula_weight         1142.06
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-10-12
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2016-10-12 deposited with the CCDC.
2017-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                75.059(3)
_cell_angle_beta                 80.399(2)
_cell_angle_gamma                63.273(3)
_cell_formula_units_Z            2
_cell_length_a                   9.8419(3)
_cell_length_b                   9.9715(3)
_cell_length_c                   17.3201(5)
_cell_measurement_reflns_used    12501
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      29.2810
_cell_measurement_theta_min      3.2720
_cell_volume                     1464.29(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -15.00   87.00   1.0000    1.5400
omega____ theta____ kappa____ phi______ frames
    -       11.1655   77.0000    0.0000 102

  2 omega  -17.00   82.00   1.0000    1.5400
omega____ theta____ kappa____ phi______ frames
    -       11.1655   57.0000 -120.0000 99

  3 omega  -18.00   52.00   1.0000    1.5400
omega____ theta____ kappa____ phi______ frames
    -       11.1655  -99.0000 -150.0000 70

  4 omega  -19.00   52.00   1.0000    1.5400
omega____ theta____ kappa____ phi______ frames
    -       11.1655  -99.0000  -30.0000 71

  5 omega   -4.00   63.00   1.0000    1.5400
omega____ theta____ kappa____ phi______ frames
    -       11.1655 -118.0000   68.0264 67

  6 omega  -13.00   84.00   1.0000    1.5400
omega____ theta____ kappa____ phi______ frames
    -       11.1655   38.0000  150.0000 97

  7 omega  -56.00   39.00   1.0000    1.5400
omega____ theta____ kappa____ phi______ frames
    -       11.1655  -57.0000   90.0000 95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0358578000
_diffrn_orient_matrix_UB_12      0.0398184000
_diffrn_orient_matrix_UB_13      -0.0366128000
_diffrn_orient_matrix_UB_21      0.0707039000
_diffrn_orient_matrix_UB_22      -0.0335085000
_diffrn_orient_matrix_UB_23      -0.0214983000
_diffrn_orient_matrix_UB_31      -0.0157696000
_diffrn_orient_matrix_UB_32      -0.0626109000
_diffrn_orient_matrix_UB_33      -0.0003172000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0760
_diffrn_reflns_av_unetI/netI     0.0565
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21486
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.853
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    13.122
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17045
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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    2.590
_exptl_crystal_description       block
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.180
_refine_diff_density_min         -2.407
_refine_diff_density_rms         0.249
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         5737
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0354
_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^)+(0.0344P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0769
_refine_ls_wR_factor_ref         0.0808
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5199
_reflns_number_total             5737
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02933k2.cif
_cod_data_source_block           exp_682
_cod_original_cell_volume        1464.30(8)
_cod_database_code               1547174
_shelxl_version_number           2013-4
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C17A) = Uanis(C17B)
3. Others
 Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(H17C)=1-FVAR(1)
 Sof(C17B)=Sof(H17D)=Sof(H17E)=Sof(H17F)=FVAR(1)
 Fixed Sof: H16A(0.5) H16B(0.5) H16C(0.5) H16D(0.5)
4.a Ternary CH refined with riding coordinates:
 C14(H14)
4.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C16(H16A,H16B), C16(H16C,H16D)
4.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C20(H20), C21(H21)
4.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C25(H25A,H25B,H25C), C17A(H17A,H17B,H17C), C17B(H17D,
 H17E,H17F)
;
_olex2_date_sample_data_collection 2014-10-27
_olex2_date_sample_submission    1414368000
_olex2_exptl_crystal_mounting_method 'Nylon Loop'
_olex2_submission_original_sample_id xstr0308
_olex2_submission_special_instructions 'No special instructions were received'