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_7052429
_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 H10 N2 O20 Os6'
_chemical_formula_weight         1907.64
_chemical_name_systematic        'Compound 7'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 105.13(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.211(4)
_cell_length_b                   19.277(4)
_cell_length_c                   19.435(3)
_cell_measurement_temperature    150(2)
_cell_volume                     4054.6(18)
_computing_molecular_graphics    'SHELXTL-PLUS (Siemens, 1991)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL-PLUS (Siemens, 1991)'
_diffrn_ambient_temperature      150(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  0.1145
_diffrn_reflns_av_sigmaI/netI    0.2232
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5609
_diffrn_reflns_theta_max         22.54
_diffrn_reflns_theta_min         2.63
_diffrn_standards_decay_%        -2
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    18.812
_exptl_absorpt_correction_T_max  0.152
_exptl_absorpt_correction_T_min  0.124
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    3.125
_exptl_crystal_description       Block
_exptl_crystal_F_000             3376
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.307
_refine_diff_density_min         -2.261
_refine_diff_density_rms         0.520
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.023
_refine_ls_goodness_of_fit_obs   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         5289
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.174
_refine_ls_restrained_S_obs      1.100
_refine_ls_R_factor_all          0.1858
_refine_ls_R_factor_obs          0.0636
_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^)+(0.0562P)^2^+44.7795P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1995
_refine_ls_wR_factor_obs         0.1342
_reflns_number_observed          2831
_reflns_number_total             5294
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b412578a.txt
_cod_data_source_block           pr9701
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w==1/[\s^2^(Fo^2^)+(0.0562P)^2^+44.7795P] 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^)+(0.0562P)^2^+44.7795P] where
P==(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7052429