Transformation of dimethyl acetylenedicarboxylate to bis(methylcarboxylate)vinylidene at a diruthenium centre: unprecedented 1,2-migration of a CO2Me group
King, Philip J.; Knox, Selby A. R.; Legge, Matthew S.; Orpen, A. Guy; Wilkinson, Jon N.; Hill, E. Alexander; Journal of the Chemical Society, Dalton Transactions  (2000) 1547–; doi:10.1039/b001666g

data_7009524
_publ_section_title
;
 Transformation of dimethyl acetylenedicarboxylate to
 bis(methylcarboxylate)vinylidene at a diruthenium centre:
 unprecedented 1,2-migration of a CO2Me group
;
_journal_issue                   10
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1547
_journal_paper_doi               10.1039/b001666g
_journal_year                    2000
_chemical_formula_sum            'C22 H20 F6 O3 Ru2'
_chemical_formula_weight         648.52
_chemical_name_systematic
;
 ?
;
_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                77.990(15)
_cell_angle_beta                 83.95(2)
_cell_angle_gamma                63.96(2)
_cell_formula_units_Z            2
_cell_length_a                   8.784(2)
_cell_length_b                   8.853(2)
_cell_length_c                   16.052(3)
_cell_measurement_reflns_used    63
_cell_measurement_temperature    173(2)
_cell_volume                     1096.9(5)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SHELXTL'
_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      173(2)
_diffrn_measurement_device       'Siemens SMART CCD area detector'
_diffrn_measurement_method       'Frames each covering 0.3 deg in \w'
_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  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11237
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.58
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.450
_exptl_absorpt_correction_T_max  0.801
_exptl_absorpt_correction_T_min  0.669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 G. M. Sheldrick. 
 SADABS: A program for absorption correction with the Siemens SMART 
system; 
 University of G\"ottingen: Germany, 1996.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.963
_exptl_crystal_density_method    none
_exptl_crystal_description       plate
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_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.934
_refine_ls_goodness_of_fit_obs   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         4949
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.934
_refine_ls_restrained_S_obs      1.011
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_obs          0.0211
_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^)+(0.0180P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0453
_refine_ls_wR_factor_obs         0.0435
_reflns_number_observed          3947
_reflns_number_total             4949
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b001666g.txt
_cod_data_source_block           7
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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^)+(0.0180P)^2^+0.0000P] 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^)+(0.0180P)^2^+0.0000P] 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        1096.9(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7009524