Synthesis, molecular structure, and reactivity of allenylideneosmium complexes of the half-sandwich-type
Birgit Weberndörfer; Helmut Werner; J. Chem. Soc., Dalton Trans.  (2002) 1479–1486; doi:10.1039/b108992g

data_7011197
_publ_section_title
;
 Synthesis, molecular structure, and reactivity of allenylideneosmium
 complexes of the half-sandwich-type
;
_journal_issue                   7
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              1479
_journal_page_last               1486
_journal_paper_doi               10.1039/b108992g
_journal_year                    2002
_chemical_formula_sum            'C29 H37 Cl F6 O Os P2'
_chemical_formula_weight         803.18
_chemical_name_systematic
; 
? 
;
_chemical_temperature_decomposition 145
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.362(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.164(3)
_cell_length_b                   16.6152(19)
_cell_length_c                   18.957(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     3138.7(15)
_computing_cell_refinement       'CAD4 (Enraf-Nonius)'
_computing_data_collection       'CAD4 (Enraf-Nonius)'
_computing_data_reduction        'BEGIN (SDP)'
_computing_molecular_graphics    'ZORTEP (Zsolnai)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CAD4 (Enraf-Nonius)'
_diffrn_measurement_method       omega-theta
_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  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0514
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5943
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.04
_diffrn_standards_decay_%        0.7
_diffrn_standards_interval_count 3600
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    4.307
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
empirical absorption correction by psi-scans from 6 reflections 
with chi-angles near 90 degrees
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.790
_refine_diff_density_min         -0.686
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         5525
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0186P)^2^+7.2093P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0650
_refine_ls_wR_factor_ref         0.0748
_reflns_number_gt                4168
_reflns_number_total             5525
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b108992g.txt
_cod_data_source_block           bw5wb
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_temperature_decomposition' since the value had been '145
(dec.)'. The value '145 (dec.)' was changed to '145'.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_cell_volume        3138.8(15)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7011197