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_4307457
_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_formula_moiety         'C31 H46 Cl4 N4 O0 Rh2'
_chemical_formula_sum            'C31 H46 Cl4 N4 O0 Rh2'
_chemical_formula_weight         822.34
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2006-09-05T09:09:04-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 99.136(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.623(3)
_cell_length_b                   14.176(4)
_cell_length_c                   13.315(4)
_cell_measurement_reflns_used    3973
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.03
_cell_measurement_theta_min      2.43
_cell_volume                     1793.3(9)
_computing_cell_refinement       'Siemens SAINT (Siemens, 1995)'
_computing_data_collection       'Siemens SMART (Siemens, 1995)'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    xtal
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    xtal
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device_type
;
Bruker SMART CCD diffractometer
;
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1008
_diffrn_reflns_av_unetI/netI     0.1047
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13473
_diffrn_reflns_theta_full        26
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    1.244
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  .60
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS; Sheldrick, 1996
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             836
_exptl_crystal_size_max          .35
_exptl_crystal_size_mid          .25
_exptl_crystal_size_min          .03
_refine_diff_density_max         4.76
_refine_diff_density_min         -0.991
_refine_diff_density_rms         0.319
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.09
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         3641
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.09
_refine_ls_R_factor_all          0.1449
_refine_ls_R_factor_gt           0.108
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.279
_refine_ls_wR_factor_ref         0.299
_reflns_number_gt                2500
_reflns_number_total             3641
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic061928gsi20061205_040617_2.cif
_cod_data_source_block           cp3cgn
_cod_original_sg_symbol_Hall     -p_2yb
_cod_database_code               4307457