Rhodium(I) and Iridium(I) Complexes with Bidentate Phosphine−Pyrazolyl Ligands: Highly Efficient Catalysts for the Hydroamination Reaction
Field, Leslie D.; Messerle, Barbara A.; Vuong, Khuong Q.; Turner, Peter; Failes, Tim; Organometallics 26 (2007) 2058–; doi:10.1021/om070057v

data_4073083
_publ_section_title
;
 Rhodium(I) and Iridium(I) Complexes with Bidentate
 Phosphine&#x2212;Pyrazolyl Ligands:&#x00A0; Highly Efficient Catalysts
 for the Hydroamination Reaction
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              2058
_journal_paper_doi               10.1021/om070057v
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C51 H53 B Ir N2 P'
_chemical_formula_weight         927.93
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 104.074(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.923(4)
_cell_length_b                   9.3077(16)
_cell_length_c                   22.399(4)
_cell_measurement_reflns_used    993
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.67
_cell_volume                     4231.2(13)
_computing_cell_refinement       'SAINT (Bruker,1995)'
_computing_data_collection       'SMART (Bruker,1995)'
_computing_data_reduction        'SAINT and XPREP (Bruker 1995)'
_computing_molecular_graphics
;
  teXsan for Windows (MSC, 1997) 
  xtal 3.6 (Hall,du Boulay, D.J. & Olthof-Hazekamp, R. 1999)
  ORTEPII  (Johnson,C.K., 1976). 
  WinGX (Farrugia, 1999)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, et. al. 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_crystal_treatment
;
attached with Exxon Paratone N, to a short length 
of fibre supported on a thin piece of copper wire 
inserted in a copper mounting pin.  The crystal was 
quenched in a cold nitrogen gas stream from an 
Oxford Cryosystems Cryostream. 
;
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_sigmaI/netI    0.0223
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            43524
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.87
_diffrn_standards_decay_%        0.14
_diffrn_standards_number         495
_exptl_absorpt_coefficient_mu    3.231
_exptl_absorpt_correction_T_max  0.657
_exptl_absorpt_correction_T_min  0.309
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
  Gaussian (Coppens et al., 1965) 
  XPREP  (Bruker, 1995)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.509
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.143
_refine_diff_density_max         0.884
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.215
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         10339
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.215
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0209
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.02P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0465
_refine_ls_wR_factor_ref         0.0475
_reflns_number_gt                8858
_reflns_number_total             10339
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om070057vsi20070118_104031.cif
_cod_data_source_block           bam12
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Gaussian' changed to
'gaussian' 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        4231.0(13)
_cod_original_sg_symbol_H-M      'P 21/n     '
_cod_database_code               4073083