Reactions of Electron-Deficient Triosmium Clusters with Diazomethane: Electrochemical Properties and Computational Studies of Charge Distribution
Mottalib, Md. Abdul; Begum, Noorjahan; Abedin, S. M. Tareque; Akter, Tahmina; Kabir, Shariff E.; Miah, Md. Arzu; Rokhsana, Dalia; Rosenberg, Edward; Hossain, G. M. Golzar; Hardcastle, Kenneth I.; Organometallics 24 (2005) 4747–; doi:10.1021/om0503794

data_4075968
_publ_section_title
;
 Reactions of Electron-Deficient Triosmium Clusters with
 Diazomethane:&#x00A0; Electrochemical Properties and Computational
 Studies of Charge Distribution
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              4747
_journal_paper_doi               10.1021/om0503794
_journal_volume                  24
_journal_year                    2005
_chemical_formula_moiety         'C20 H11 N O9 Os3'
_chemical_formula_sum            'C20 H11 N O9 Os3'
_chemical_formula_weight         979.90
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.764(3)
_cell_angle_beta                 90.929(3)
_cell_angle_gamma                100.978(3)
_cell_formula_units_Z            2
_cell_length_a                   9.6788(12)
_cell_length_b                   10.4164(14)
_cell_length_c                   11.5639(15)
_cell_measurement_reflns_used    3077
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.44
_cell_volume                     1122.8(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0360
_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       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11751
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    16.985
_exptl_absorpt_correction_T_max  0.1770
_exptl_absorpt_correction_T_min  0.1192
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10, Sheldrick 2003'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.899
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.693
_refine_diff_density_min         -2.272
_refine_diff_density_rms         0.206
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         5571
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0243
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0297P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0578
_refine_ls_wR_factor_ref         0.0589
_reflns_number_gt                5146
_reflns_number_total             5571
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0503794si20050512_071200.cif
_cod_data_source_block           10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4075968