Rearrangement and Scission of Terminal Alkynes in Dimolybdenum Complexes on Reaction with Ruthenium Carbonyl: Formation of Trinuclear Vinylidene and Hexanuclear Bis(alkylidyne) Clusters
Adams, Harry; Gill, Louise J.; Morris, Michael J.; Organometallics 15 (1996) 4182–; doi:10.1021/om960235c

data_4078333
_publ_section_title
;
 Rearrangement and Scission of Terminal Alkynes in Dimolybdenum Complexes
 on Reaction with Ruthenium Carbonyl:&#x00A0; Formation of Trinuclear
 Vinylidene and Hexanuclear Bis(alkylidyne) Clusters
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              4182
_journal_paper_doi               10.1021/om960235c
_journal_volume                  15
_journal_year                    1996
_chemical_formula_sum            'C20 H14 Mo2 O7 Ru'
_chemical_formula_weight         659.26
_chemical_name_systematic
; 
 ? 
;
_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                 96.350(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.3070(10)
_cell_length_b                   16.190(2)
_cell_length_c                   13.9550(10)
_cell_measurement_reflns_used    39
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.991
_cell_measurement_theta_min      9.736
_cell_volume                     2089.8(4)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w 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  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3435
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.93
_diffrn_standards_decay_%        7.50
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.934
_exptl_crystal_colour            'deep red'
_exptl_crystal_density_diffrn    2.095
_exptl_crystal_description       'oblong blocks'
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.722
_refine_diff_density_min         -2.711
_refine_diff_density_rms         0.337
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.274
_refine_ls_goodness_of_fit_obs   1.294
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         2715
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.274
_refine_ls_restrained_S_obs      1.294
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_obs          0.0476
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0748P)^2^+1.5741P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1225
_refine_ls_wR_factor_obs         0.1205
_reflns_number_observed          2560
_reflns_number_total             2715
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om4182.cif
_cod_data_source_block           lg123x
_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_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0748P)^2^+1.5741P] 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^)+(0.0748P)^2^+1.5741P] 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      P2(1)/n
_cod_database_code               4078333