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_7052428
_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            'C34 H8 N2 O20 Os6'
_chemical_formula_weight         1905.62
_chemical_name_systematic        'Compound 6'
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.085(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.7840(6)
_cell_length_b                   28.201(3)
_cell_length_c                   16.7970(9)
_cell_measurement_reflns_used    20039
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      2.910
_cell_volume                     4129.1(6)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection
;
"Collect" data collection software, Nonius' B.V., 1998.
;
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       CCD
_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  0.0855
_diffrn_reflns_av_sigmaI/netI    0.1112
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24123
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.66
_exptl_absorpt_coefficient_mu    18.472
_exptl_absorpt_correction_T_max  0.691
_exptl_absorpt_correction_T_min  0.565
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav Blessing (1995)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.065
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3368
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.961
_refine_diff_density_min         -2.303
_refine_diff_density_rms         0.311
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.017(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1117
_refine_ls_number_reflns         12818
_refine_ls_number_restraints     631
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0495
_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^)+(0.0433P)^2^] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1116
_reflns_number_gt                10371
_reflns_number_total             12818
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b412578a.txt
_cod_data_source_block           pr0016
_cod_original_cell_volume        4129.1(5)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7052428