Molecular rearrangements of diynes coordinated to triosmium carbonyl clusters: reactions of [Os3(�-H)2(CO)10] and [Os3(CO)10(MeCN)2] with 1,4-dipyridylbuta-1,3-diyne
Clarke, Lionel P.; Cole, Jacqueline M.; Davies, John E.; French, Alexandra; Koentjoro, Olivia F.; Raithby, Paul R.; Shields, Gregory P.; New Journal of Chemistry 29 (2005) 145–; doi:10.1039/b412578a

data_7052426
_publ_section_title
;
 Molecular rearrangements of diynes coordinated to triosmium carbonyl
 clusters: reactions of [Os3(&#xFFFD;-H)2(CO)10] and [Os3(CO)10(MeCN)2]
 with 1,4-dipyridylbuta-1,3-diyne
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              145
_journal_paper_doi               10.1039/b412578a
_journal_volume                  29
_journal_year                    2005
_chemical_formula_sum            'C23 H10 N2 O9 Os3'
_chemical_formula_weight         1028.93
_chemical_name_systematic        'Compound 3'
_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
_cell_angle_alpha                107.27(2)
_cell_angle_beta                 102.64(4)
_cell_angle_gamma                85.36(3)
_cell_formula_units_Z            2
_cell_length_a                   10.250(5)
_cell_length_b                   14.515(4)
_cell_length_c                   8.843(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_volume                     1225.7(8)
_computing_cell_refinement
'Rigaku AFC5R diffractometer control software'
_computing_data_collection
'Rigaku AFC5R diffractometer control software'
_computing_data_reduction
'Rigaku AFC5R diffractometer control software'
_computing_molecular_graphics    'SHELXTL-PLUS (Sheldrick, 1991)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Rigaku AFC5R four-circle diffractometer'
_diffrn_measurement_method       '\w/2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0986
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7473
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         3.50
_diffrn_standards_decay_%        2
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    15.567
_exptl_absorpt_correction_T_max  0.288
_exptl_absorpt_correction_T_min  0.171
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    2.788
_exptl_crystal_description       Prism
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.214
_refine_diff_density_min         -1.867
_refine_diff_density_rms         0.295
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.012
_refine_ls_goodness_of_fit_obs   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         5617
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_restrained_S_obs      1.056
_refine_ls_R_factor_all          0.0982
_refine_ls_R_factor_obs          0.0406
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w==1/[\s^2^(Fo^2^)+(0.0408P)^2^+1.3110P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1068
_refine_ls_wR_factor_obs         0.0891
_reflns_number_observed          3738
_reflns_number_total             5621
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            b412578a.txt
_cod_data_source_block           pr9615
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w==1/[\s^2^(Fo^2^)+(0.0408P)^2^+1.3110P] where P==(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w==1/[\s^2^(Fo^2^)+(0.0408P)^2^+1.3110P] where P==(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1225.7(7)
_cod_database_code               7052426