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_1547172
_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         'C24 H15 N O13 Os3 S'
_chemical_formula_sum            'C24 H15 N O13 Os3 S'
_chemical_formula_weight         1128.03
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-10-11
_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                78.130(3)
_cell_angle_beta                 74.717(3)
_cell_angle_gamma                81.572(3)
_cell_formula_units_Z            2
_cell_length_a                   10.2449(3)
_cell_length_b                   11.0705(4)
_cell_length_c                   13.4872(4)
_cell_measurement_reflns_used    11971
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      29.1140
_cell_measurement_theta_min      3.5080
_cell_volume                     1437.09(8)
_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)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -44.00   39.00   1.0000    1.5750
omega____ theta____ kappa____ phi______ frames
    -       11.0092  -57.0000   60.0000 83

  2 omega  -16.00   52.00   1.0000    1.5750
omega____ theta____ kappa____ phi______ frames
    -       11.0092  -99.0000  -30.0000 68

  3 omega  -25.00   91.00   1.0000    1.5750
omega____ theta____ kappa____ phi______ frames
    -       11.0092   19.0000  150.0000 116

  4 omega  -19.00   57.00   1.0000    1.5750
omega____ theta____ kappa____ phi______ frames
    -       11.0092   77.0000  -30.0000 76

  5 omega  -13.00   85.00   1.0000    1.5750
omega____ theta____ kappa____ phi______ frames
    -       11.0092   38.0000 -120.0000 98

  6 omega  -59.00   44.00   1.0000    1.5750
omega____ theta____ kappa____ phi______ frames
    -       11.0092  -77.0000 -180.0000 103
;
_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      0.0715527000
_diffrn_orient_matrix_UB_12      0.0015391000
_diffrn_orient_matrix_UB_13      -0.0162398000
_diffrn_orient_matrix_UB_21      0.0083241000
_diffrn_orient_matrix_UB_22      -0.0651075000
_diffrn_orient_matrix_UB_23      0.0018542000
_diffrn_orient_matrix_UB_31      -0.0034693000
_diffrn_orient_matrix_UB_32      0.0093005000
_diffrn_orient_matrix_UB_33      -0.0529066000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19242
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.899
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    13.369
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.19410
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.607
_exptl_crystal_description       block
_exptl_crystal_F_000             1028
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.039
_refine_diff_density_min         -2.619
_refine_diff_density_rms         0.286
_refine_ls_extinction_coef       0.00116(13)
_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   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         5630
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0348
_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^)+(0.0451P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.0862
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5159
_reflns_number_total             5630
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02933k2.cif
_cod_data_source_block           xstr0280
_cod_database_code               1547172
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'Os3 C24 O13 H15 S1 N1'
_chemical_oxdiff_usercomment     AH-146C
_reflns_odcompleteness_completeness 99.83
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C21(H21)
2.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C23(H23A,H23B)
2.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C13(H13), C14(H14), C15(H15)
2.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C24(H24A,H24B,H24C)
;
_olex2_date_sample_data_collection 2014-08-29
_olex2_date_sample_submission    1409266800
_olex2_exptl_crystal_mounting_method 'Nylon Loop'
_olex2_submission_original_sample_id xstr0280
_olex2_submission_special_instructions 'No special instructions were received'