Synthesis, Reactivity, Spectroscopic Characterization, X-ray Structures, PGSE, and NOE NMR Studies of (η5-C5Me5)-Rhodium and -Iridium Derivatives Containing Bis(pyrazolyl)alkane Ligands
Claudio Pettinari; Riccardo Pettinari; Fabio Marchetti; Alceo Macchioni; Daniele Zuccaccia; Brian W. Skelton; Allan H. White; Inorganic Chemistry 46 (2007) 896–906; doi:10.1021/ic061928g

data_4307463
_publ_contact_author_address
;
   Department of Chemistry
   University of Western Australia
   35 Stirling Highway
   Crawley
   Western Australia 6009
   Australia
;
_publ_contact_author_email       bws@crystal.uwa.edu.au
_publ_contact_author_fax         (+61)_08_6488_1118
_publ_contact_author_name        'Skelton, B. W.'
_publ_contact_author_phone       (+61)_08_6488_7107
_publ_section_title
;
Synthesis, Reactivity, Spectroscopic Characterization, X-ray Structures,
PGSE, and NOE NMR Studies of (\h5-C5Me5)-Rhodium and -Iridium Derivatives
Containing Bis(pyrazolyl)alkane Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              896
_journal_page_last               906
_journal_paper_doi               10.1021/ic061928g
_journal_volume                  46
_journal_year                    2007
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C17 H25 N4 O Rh, 2(C F3 O3 S)'
_chemical_formula_sum            'C19 H25 F6 N4 O7 Rh S2'
_chemical_formula_weight         702.46
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2006-08-27T14:16:20-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 105.891(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.292(3)
_cell_length_b                   10.2940(10)
_cell_length_c                   14.626(4)
_cell_measurement_reflns_used    27335
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      38.0994
_cell_measurement_theta_min      2.5319
_cell_volume                     2648.8(9)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.30.5 (release 12-06-2006 CrysAlis171 .NET)
        (compiled Jun 12 2006,17:01:16)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.30.5 (release 12-06-2006 CrysAlis171 .NET)
        (compiled Jun 12 2006,17:01:16)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.30.5 (release 12-06-2006 CrysAlis171 .NET)
        (compiled Jun 12 2006,17:01:16)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0009
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device_type
;
 Oxford Diffraction Xcalibur diffractometer
;
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0377539961
_diffrn_orient_matrix_UB_12      -0.0205282127
_diffrn_orient_matrix_UB_13      -0.0220633673
_diffrn_orient_matrix_UB_21      0.0123962
_diffrn_orient_matrix_UB_22      -0.0655935546
_diffrn_orient_matrix_UB_23      0.0030067828
_diffrn_orient_matrix_UB_31      -0.0069783139
_diffrn_orient_matrix_UB_32      -0.0056516857
_diffrn_orient_matrix_UB_33      0.0451941197
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            44821
_diffrn_reflns_theta_full        38.
_diffrn_reflns_theta_max         38.
_diffrn_reflns_theta_min         2.54
_exptl_absorpt_coefficient_mu    0.891
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.93099
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.30.5 (release 12-06-2006 CrysAlis171 .NET)
        (compiled Jun 12 2006,17:01:16)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       hexagonal_prism
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.19
_refine_diff_density_max         2.909
_refine_diff_density_min         -0.753
_refine_diff_density_rms         0.09
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         13535
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0314P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0579
_refine_ls_wR_factor_ref         0.0598
_reflns_number_gt                11410
_reflns_number_total             13535
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic061928gsi20061205_040617_8.cif
_cod_data_source_block           cprhtf
_cod_original_sg_symbol_Hall     c_-2yc
_cod_database_code               4307463