New Rhodium(I) and Iridium(I) Complexes Containing Mixed Pyrazolyl–1,2,3-Triazolyl Ligands As Catalysts for Hydroamination
Hua, Carol; Vuong, Khuong Q.; Bhadbhade, Mohan; Messerle, Barbara A.; Organometallics 31 (2012) 1790–; doi:10.1021/om201171b

data_4076399
_publ_section_title
;
 New Rhodium(I) and Iridium(I) Complexes Containing Mixed
 Pyrazolyl--1,2,3-Triazolyl Ligands As Catalysts for Hydroamination
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1790
_journal_paper_doi               10.1021/om201171b
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C45 H45 B N5 Rh'
_chemical_formula_weight         769.58
_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                69.653(2)
_cell_angle_beta                 77.243(2)
_cell_angle_gamma                87.569(2)
_cell_formula_units_Z            2
_cell_length_a                   9.3525(4)
_cell_length_b                   13.3346(6)
_cell_length_c                   16.0237(7)
_cell_measurement_reflns_used    9967
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.506
_cell_measurement_theta_min      2.235
_cell_volume                     1826.12(14)
_computing_cell_refinement       '<i>APEX2 </i>(Bruker, 2007)'
_computing_data_collection       '<i>APEX2 </i>(Bruker, 2007)'
_computing_data_reduction        '<i>APEX2 </i>(Bruker, 2007)'
_computing_molecular_graphics    '<i>SHELXTL-Plus</i> (Sheldrick, 2008)'
_computing_structure_refinement  '<i>SHELXL-97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS-97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker kappa APEXII CCD Diffractometer'
_diffrn_measurement_method       '\f scans, and \w scans with \k offsets'
_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  0.0460
_diffrn_reflns_av_sigmaI/netI    0.0438
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25386
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.69
_exptl_absorpt_coefficient_mu    0.508
_exptl_absorpt_correction_T_max  0.9610
_exptl_absorpt_correction_T_min  0.8494
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2001)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plates
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.573
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         6390
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0201P)^2^+1.5585P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0632
_refine_ls_wR_factor_ref         0.0670
_reflns_number_gt                5500
_reflns_number_total             6390
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201171b_si_002.cif
_cod_data_source_block           khuong11_p1bar
_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.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' 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_database_code               4076399