Variable coordination of amine functionalised N-heterocyclic carbene ligands to Ru, Rh and Ir: C-H and N-H activation and catalytic transfer hydrogenation.
Cross, Warren B.; Daly, Christopher G.; Boutadla, Youcef; Singh, Kuldip; Dalton transactions (Cambridge, England : 2003) 40 (2011) 9722–9730; doi:10.1039/c1dt10753d

data_7016802
_publ_section_title
;
 Variable coordination of amine functionalised N-heterocyclic carbene
 ligands to Ru, Rh and Ir: C-H and N-H activation and catalytic
 transfer hydrogenation.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9722
_journal_page_last               9730
_journal_paper_doi               10.1039/c1dt10753d
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C22 H30 I Ir N3, C2 F3 O2,5C5H12'
_chemical_formula_sum            'C49 H90 F3 I Ir N3 O2'
_chemical_formula_weight         1129.34
_chemical_name_common            '[Cp*Ir(C,NH2)I][CF3CO2] (8)'
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 110.741(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.957(3)
_cell_length_b                   10.360(2)
_cell_length_c                   21.186(4)
_cell_measurement_reflns_used    657
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.402
_cell_measurement_theta_min      2.349
_cell_volume                     3480.6(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Apex 2000 CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.1501
_diffrn_reflns_av_sigmaI/netI    0.1704
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            26753
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    4.795
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.539
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
absorption correction based on 4559 reflections(SADABS);Rint 0.1338 before
correction and 0.0635 after.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.155
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2312
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.991
_refine_diff_density_min         -1.925
_refine_diff_density_rms         0.200
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.795
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         6829
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.795
_refine_ls_R_factor_all          0.0949
_refine_ls_R_factor_gt           0.0541
_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^)+(0.0315P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1052
_refine_ls_wR_factor_ref         0.1136
_reflns_number_gt                3745
_reflns_number_total             6829
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10753d.txt
_cod_data_source_block           11026
_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        3480.6(12)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7016802