R-Group reversal of isomer stability for RuH(X)L2(CCHR) vs. Ru(X)L2(CCH2R): access to four-coordinate ruthenium carbenes and carbynes
Coalter, Joseph N.; Bollinger, John C.; Eisenstein, Odile; Caulton, Kenneth G.; New Journal of Chemistry 24 (2000) 925–; doi:10.1039/b006971j

data_7051375
_publ_section_title
;
 R-Group reversal of isomer stability for RuH(X)L2(CCHR) vs.
 Ru(X)L2(CCH2R): access to four-coordinate ruthenium carbenes and
 carbynes
;
_journal_issue                   12
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              925
_journal_paper_doi               10.1039/b006971j
_journal_volume                  24
_journal_year                    2000
_chemical_formula_moiety         'C31 H52 O P2 Ru'
_chemical_formula_sum            'C31 H52 O P2 Ru'
_chemical_formula_weight         603.74
_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-97
_cell_angle_alpha                93.353(8)
_cell_angle_beta                 92.003(8)
_cell_angle_gamma                97.681(11)
_cell_formula_units_Z            2
_cell_length_a                   8.884(3)
_cell_length_b                   11.352(4)
_cell_length_c                   16.041(6)
_cell_measurement_reflns_used    511
_cell_measurement_temperature    111(2)
_cell_measurement_theta_max      35.41
_cell_measurement_theta_min      2.85
_cell_volume                     1599.0(10)
_computing_cell_refinement       'SMART (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction
'SAINT (Bruker, 1999), Gemini (Bruker 2000), XTEL (local package)'
_computing_molecular_graphics    'XTEL (local package)'
_computing_publication_material  'XTEL (local package)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      111(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
'   0.30 degree frames measured for  10.13 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0970
_diffrn_reflns_av_sigmaI/netI    0.1510
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            68114
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        -0.7
_diffrn_standards_interval_time  614
_diffrn_standards_number         94
_exptl_absorpt_coefficient_mu    0.611
_exptl_absorpt_correction_T_max  .983
_exptl_absorpt_correction_T_min  .907
_exptl_absorpt_correction_type   'numerical (Gaussian)'
_exptl_absorpt_process_details   'XPREP 5.10 (Bruker, 1997)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             640
_exptl_crystal_size_max          .16
_exptl_crystal_size_mid          .15
_exptl_crystal_size_min          .03
_refine_diff_density_max         1.574
_refine_diff_density_min         -1.183
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.911
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         19002
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.911
_refine_ls_R_factor_all          0.0912
_refine_ls_R_factor_gt           0.0553
_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
   [\s^2^(Fo^2^)+(0.0500Fo^2^)^2^]^-1^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1326
_refine_ls_wR_factor_ref         0.1401
_reflns_number_gt                11132
_reflns_number_total             19002
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            b006971j.txt
_cod_data_source_block           00092
_cod_original_cell_volume        1598.9(10)
_cod_database_code               7051375