Crabtree's catalyst revisited; ligand effects on stability and durability
Xu, Yingjian; Mingos, D. Michael P.; Brown, John M.; Chemical Communications (Cambridge, United Kingdom)  (2008) 199–201; doi:10.1039/b711979h

data_7102793
_publ_section_title
;
 Crabtree's catalyst revisited; ligand effects on stability and durability
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   2
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              199
_journal_page_last               201
_journal_paper_doi               10.1039/b711979h
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         ' C35 H56 Ir N P, F6 P '
_chemical_formula_sum            'C35 H56 F6 Ir N P2'
_chemical_formula_weight         858.99
_chemical_name_common
;Iridium(1+)((1,2,5,6-eta)(1,5-COD)(5,6,7,8-
THQ)(P(Cyclohexyl)3)PF6(1-).
;
_chemical_name_systematic
;
Iridium(1+)[(1,2,5,6-eta)(1,5-COD](5,6,7,8-THQ)(P(Cyclohexyl)3)PF6(1-).
;
_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     heavy
_cell_angle_alpha                97.6584(8)
_cell_angle_beta                 103.4087(9)
_cell_angle_gamma                99.2889(11)
_cell_formula_units_Z            2
_cell_length_a                   10.0545(2)
_cell_length_b                   11.8176(2)
_cell_length_c                   15.5293(3)
_cell_measurement_reflns_used    25277
_cell_measurement_temperature    120
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     1743.13(6)
_computing_cell_refinement
;
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_data_collection
;
KappaCCD software 'Collect' (Nonius, 2000)
;
_computing_data_reduction
;
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_publication_material
;
CRYSTALS (Watkin et al, 2001)
;
_computing_structure_refinement
;
CRYSTALS (Watkin et al, 2001)
;
_computing_structure_solution    'CRYSTALS (Watkin et al, 2001)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type
;
Nonius KappaCCD
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.062
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25277
_diffrn_reflns_theta_full        27.493
_diffrn_reflns_theta_max         27.493
_diffrn_reflns_theta_min         5.098
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.980
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_exptl_crystal_colour            ' orange-red '
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_description       ' plate '
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_exptl_crystal_thermal_history
;
The material was crystallised at ambient temperature. A suitable crystal
was cooled to 120K at a rate of 120 K hr^-1^ for single-crystal X-ray
diffraction analysis.
;
_refine_diff_density_max         2.87
_refine_diff_density_min         -3.33
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0801
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         6887
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.006071
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
0.986 0.255 0.632
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0538
_refine_ls_wR_factor_gt          0.0489
_refine_ls_wR_factor_ref         0.0489
_reflns_limit_h_max              12
_reflns_limit_h_min              -13
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                6887
_reflns_number_total             7896
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            b711979h.txt
_cod_data_source_block           arc1365
_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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        ' C35 H56 F6 Ir N P2 '
_cod_database_code               7102793