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_4078334
_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            'C27 H18 Cl2 Mo2 O12 Ru4'
_chemical_formula_weight         1201.47
_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                 91.810(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.126(3)
_cell_length_b                   14.672(2)
_cell_length_c                   15.196(2)
_cell_measurement_reflns_used    39
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.997
_cell_measurement_theta_min      9.928
_cell_volume                     3370.7(9)
_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  0.0233
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5365
_diffrn_reflns_theta_max         22.51
_diffrn_reflns_theta_min         1.87
_diffrn_standards_decay_%        20.78
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.685
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.368
_exptl_crystal_description       'oblong blocks'
_exptl_crystal_F_000             2280
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.683
_refine_diff_density_min         -2.035
_refine_diff_density_rms         0.338
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.224
_refine_ls_goodness_of_fit_obs   1.262
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         4315
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.227
_refine_ls_restrained_S_obs      1.262
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_obs          0.0384
_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^)+(0.0564P)^2^+2.9796P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1018
_refine_ls_wR_factor_obs         0.0985
_reflns_number_observed          3861
_reflns_number_total             4316
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om4182.cif
_cod_data_source_block           lg514
_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.

'_geom_bond_publ_flag' value 'Y' changed to 'y'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (19
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (48 times).

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^)+(0.0564P)^2^+2.9796P] 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^)+(0.0564P)^2^+2.9796P] 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               4078334