Carbon-Carbon Double Bond Formation from Two o-Methyl Groups in Osmium Phosphine Complexes
Walter Baratta; Eberhardt Herdtweck; Paolo Martinuzzi; Pierluigi Rigo; Organometallics 20 (2001) 305–308; doi:10.1021/om000593m

data_4063190
_publ_section_title
;
 Carbon-Carbon Double Bond Formation from Two o-Methyl Groups in Osmium
 Phosphine Complexes
;
_journal_name_full               Organometallics
_journal_page_first              305
_journal_page_last               308
_journal_paper_doi               10.1021/om000593m
_journal_volume                  20
_journal_year                    2001
_chemical_formula_moiety         '(C60 H52 Cl Os P3), (C H2 Cl2)'
_chemical_formula_sum            'C61 H54 Cl3 Os P3'
_chemical_formula_weight         1176.58
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90.375(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7810(1)
_cell_length_b                   18.9967(2)
_cell_length_c                   21.4222(2)
_cell_measurement_reflns_used    61468
_cell_measurement_temperature    163(1)
_cell_measurement_theta_max      26.35
_cell_measurement_theta_min      3.35
_cell_volume                     5201.13(8)
_computing_cell_refinement       'Denzo and HKL'
_computing_data_collection       'Kappa CCD (Nonius)'
_computing_data_reduction        'Denzo and HKL'
_computing_molecular_graphics    'PLATON PLUTON (Spek, 1990)'
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR-92 (Giacovazzo, 1992)'
_diffrn_ambient_temperature      163(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 18
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Kappa CCD (Nonius)'
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'NONIUS FR 591 rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.032
_diffrn_reflns_av_sigmaI/netI    0.0214
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            57109
_diffrn_reflns_reduction_process
;
 with the Kappa CCD software Scale-Pack 
;
_diffrn_reflns_theta_max         26.35
_diffrn_reflns_theta_min         3.35
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.738
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  1.000
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
 none
;
_exptl_crystal_colour            ' light green '
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       ' fragment '
_exptl_crystal_F_000             2368
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.018
_refine_diff_density_min         -1.240
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.074
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     828
_refine_ls_number_reflns         10557
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_restrained_S_obs      1.118
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0242
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          -0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0388P)^2^+5.4147P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0671
_refine_ls_wR_factor_ref         0.0658
_reflns_number_gt                9443
_reflns_number_total             10557
_reflns_threshold_expression     >2sigma(i)
_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.

'_exptl_absorpt_correction_type' value ' none ' changed to
'none' 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:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4063190