Square-Planar Bis(triisopropylstibine)(olefin)iridium(I) Complexes and Their Rearrangement to (η3-Allyl)hydridoiridium(III) Isomers
Ortmann, Dagmara A.; Gevert, Olaf; Laubender, Matthias; Werner, Helmut; Organometallics 20 (2001) 1776–; doi:10.1021/om001078r

data_4077277
_publ_section_title
;
 Square-Planar Bis(triisopropylstibine)(olefin)iridium(I) Complexes and
 Their Rearrangement to (\h3-Allyl)hydridoiridium(III) Isomers
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              1776
_journal_paper_doi               10.1021/om001078r
_journal_volume                  20
_journal_year                    2001
_chemical_formula_sum            'C21 H48 Cl Ir Sb2'
_chemical_formula_weight         771.74
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 93.631(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   42.065(10)
_cell_length_b                   8.7348(9)
_cell_length_c                   14.658(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      15.00
_cell_measurement_theta_min      10.00
_cell_volume                     5375.0(18)
_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      173(2)
_diffrn_measurement_device       'CAD4 (Enraf-Nonius)'
_diffrn_measurement_method       Omega-Theta-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  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5756
_diffrn_reflns_theta_max         27.04
_diffrn_reflns_theta_min         2.38
_diffrn_standards_decay_%        1.1
_diffrn_standards_interval_count 3600
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.145
_exptl_absorpt_correction_T_max  100.00
_exptl_absorpt_correction_T_min  89.48
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
 empirical absorption correction by psi-scans from 9 reflections 
 with chi-angles near 90 degrees
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.907
_exptl_crystal_description       prism
_exptl_crystal_F_000             2960
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.865
_refine_diff_density_min         -0.890
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.051
_refine_ls_goodness_of_fit_obs   1.051
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         5501
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_restrained_S_obs      1.051
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_obs          0.0324
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+9.0181P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0728
_refine_ls_wR_factor_obs         0.0662
_reflns_number_observed          4593
_reflns_number_total             5501
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om001078r.cif
_cod_data_source_block           6a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+9.0181P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+9.0181P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5375.0(17)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4077277