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_4307459
_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         'C21 H31 Cl N4 Rh, Cl, 1/2(C H2 Cl2)'
_chemical_formula_sum            'C21.5 H32 Cl3 N4 Rh'
_chemical_formula_weight         555.77
_chemical_name_systematic
;
 ?
;
_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_date             2006-09-06T11:43:05-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                74.662(5)
_cell_angle_beta                 82.048(5)
_cell_angle_gamma                63.242(5)
_cell_formula_units_Z            4
_cell_length_a                   12.602(4)
_cell_length_b                   13.993(5)
_cell_length_c                   17.467(6)
_cell_measurement_reflns_used    4068
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.72
_cell_measurement_theta_min      2.78
_cell_volume                     2651.7(16)
_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 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.075
_diffrn_reflns_av_unetI/netI     0.1821
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22725
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    .909
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  .57
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS; Sheldrick, 1996
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          .28
_exptl_crystal_size_mid          .17
_exptl_crystal_size_min          .06
_refine_diff_density_max         2.473
_refine_diff_density_min         -1.768
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     566
_refine_ls_number_reflns         9135
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.1778
_refine_ls_R_factor_gt           0.1042
_refine_ls_shift/su_max          0.047
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1521P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2699
_refine_ls_wR_factor_ref         0.2955
_reflns_number_gt                5235
_reflns_number_total             9135
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic061928gsi20061205_040617_4.cif
_cod_data_source_block           cprhl2
_cod_original_sg_symbol_Hall     -p_1
_cod_original_formula_sum        'C21.50 H32 Cl3 N4 Rh'
_cod_database_code               4307459