Synthesis and Protonation Studies of Cp*Os(dppe)H: Kinetic versus Thermodynamic Control
Dub, Pavel A.; Belkova, Natalia V.; Lyssenko, Konstantin A.; Silantyev, Gleb A.; Epstein, Lina M.; Shubina, Elena S.; Daran, Jean-Claude; Poli, Rinaldo; Organometallics 27 (2008) 3307–; doi:10.1021/om8000235

data_4071186
_publ_section_title
;
 Synthesis and Protonation Studies of Cp*Os(dppe)H: Kinetic versus
 Thermodynamic Control
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3307
_journal_paper_doi               10.1021/om8000235
_journal_volume                  27
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C18 H27 Br Os'
_chemical_formula_sum            'C18 H27 Br Os'
_chemical_formula_weight         513.51
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.170(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.7839(3)
_cell_length_b                   13.3233(4)
_cell_length_c                   14.1332(5)
_cell_measurement_reflns_used    11499
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      31.9
_cell_measurement_theta_min      2.8
_cell_volume                     1641.08(10)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare et al., 1997)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 8.2632
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       '\w and \f'
_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  0.0503
_diffrn_reflns_av_sigmaI/netI    0.0355
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12449
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.79
_exptl_absorpt_coefficient_mu    10.194
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.03380
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
CrysAlis RED (Oxford Diffraction, 2006)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.078
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       planar
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.82
_exptl_crystal_size_mid          0.66
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.152
_refine_diff_density_min         -3.729
_refine_diff_density_rms         0.352
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         4065
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0614P)^2^+24.0341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1112
_refine_ls_wR_factor_ref         0.1239
_reflns_number_gt                3527
_reflns_number_total             4065
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om8000235-file003.cif
_cod_data_source_block           OsBr
_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 
;
_cod_original_cell_volume        1641.08(9)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4071186