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_1547173
_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     direct
_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                75.769(2)
_cell_angle_beta                 84.515(2)
_cell_angle_gamma                84.498(2)
_cell_formula_units_Z            4
_cell_length_a                   10.0477(16)
_cell_length_b                   16.538(3)
_cell_length_c                   17.657(3)
_cell_measurement_reflns_used    5247
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.39
_cell_volume                     2823.0(8)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_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_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_unetI/netI     0.0672
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21541
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.274
_exptl_absorpt_coefficient_mu    13.610
_exptl_absorpt_correction_T_max  0.1932
_exptl_absorpt_correction_T_min  0.145703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.1880 before and 0.0526 after correction.
The Ratio of minimum to maximum transmission is 0.1457.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.654
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.786
_refine_diff_density_min         -1.890
_refine_diff_density_rms         0.273
_refine_ls_extinction_coef       0.00013(4)
_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   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     758
_refine_ls_number_reflns         10939
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0448P)^2^+4.9046P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1067
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9293
_reflns_number_total             10939
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02933k2.cif
_cod_data_source_block           str0555
_cod_original_cell_volume        2823.1(8)
_cod_database_code               1547173
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.193
_shelx_estimated_absorpt_t_min   0.066
_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:
 C24(H24), C74(H74)
2.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C26(H26A,H26B), C71(H71A,H71B), C76(H76A,H76B)
2.c Me refined with riding coordinates:
 C20(H20A,H20B,H20C), C27(H27A,H27B,H27C), C70(H70A,H70B,H70C), C77(H77A,H77B,
 H77C)
2.d Aromatic/amide H refined with riding coordinates:
 C10(H10), C13(H13), C14(H14), C15(H15), C60(H60), C63(H63), C64(H64), C65(H65)
;
_olex2_submission_special_instructions 'No special instructions were received'