Diverse Coordination Modes and Transformations of Allenes at Adjacent Iridium/Osmium Centers
MacDougall, Tiffany J.; Ferguson, Michael J.; McDonald, Robert; Cowie, Martin; Organometallics 31 (2012) 4516–; doi:10.1021/om300316h

data_4078548
_publ_section_title
;
 Diverse Coordination Modes and Transformations of Allenes at Adjacent
 Iridium/Osmium Centers
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              4516
_journal_paper_doi               10.1021/om300316h
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C57 H50 Ir O3 Os P4, C F3 O3 S, 2(C H2 Cl2)'
_chemical_formula_sum            'C60 H54 Cl4 F3 Ir O6 Os P4 S'
_chemical_formula_weight         1608.17
_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-97
_cell_angle_alpha                98.8679(12)
_cell_angle_beta                 96.8074(12)
_cell_angle_gamma                112.3778(11)
_cell_formula_units_Z            2
_cell_length_a                   11.4554(10)
_cell_length_b                   12.7418(11)
_cell_length_c                   23.037(2)
_cell_measurement_reflns_used    9962
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.16
_cell_volume                     3013.8(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF-2008 (Beurskens et al., 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_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  0.0451
_diffrn_reflns_av_sigmaI/netI    0.0629
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            26054
_diffrn_reflns_theta_full        25.30
_diffrn_reflns_theta_max         27.58
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    4.689
_exptl_absorpt_correction_T_max  0.8062
_exptl_absorpt_correction_T_min  0.1259
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1572
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
Attempts to refine peaks of residual electron density as
disordered or partial-occupancy solvent dichloromethane chlorine or
carbon atoms were unsuccessful.  The data were corrected for
disordered electron density through use of the SQUEEZE procedure
(Sluis, P. van der; Spek, A. L. Acta Crystallogr. 1990, A46, 194-201)
as implemented in PLATON (Spek, A. L. Acta Crystallogr. 1990, A46,
C34; Spek, A. L. J. Appl. Cryst. 2003, 36, 7-13.  PLATON - a
multipurpose crystallographic tool.  Utrecht University, Utrecht, The
Netherlands).  A total solvent-accessible void volume of 368.7 cubic
Angstroms with a total electron count of 120 (consistent with three
molecules of solvent dichloromethane, or 1.5 molecules per formula
unit of the IrOs complex cation) was found in the unit cell.
;
_refine_diff_density_max         2.819
_refine_diff_density_min         -2.442
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     743
_refine_ls_number_reflns         13777
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0452
_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 w=1/[\s^2^(Fo^2^)+(0.0163P)^2^+19.8901P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.0971
_reflns_number_gt                10820
_reflns_number_total             13777
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om300316h_si_003.cif
_cod_data_source_block           3-3a
_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_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_database_code               4078548