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_4307456
_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         'C17 H23 Cl Ir1 N4, Cl, H2 O'
_chemical_formula_sum            'C17 H25 Cl2 Ir N4 O'
_chemical_formula_weight         564.54
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                102.563(6)
_cell_angle_beta                 99.460(6)
_cell_angle_gamma                97.057(6)
_cell_formula_units_Z            2
_cell_length_a                   7.542(3)
_cell_length_b                   8.536(3)
_cell_length_c                   15.912(6)
_cell_measurement_reflns_used    3638
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.02
_cell_measurement_theta_min      2.48
_cell_volume                     972.8(6)
_computing_cell_refinement       'Siemens SAINT (Siemens, 1995)'
_computing_data_collection       'Siemens SMART (Siemens, 1995)'
_computing_data_reduction        xtal
_computing_molecular_graphics    xtal
_computing_publication_material  'xtal BONDLA CIFIO'
_computing_structure_refinement  xtal
_computing_structure_solution    xtal
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device_type
;
Bruker SMART CCD diffractometer
;
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_detector       'CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .052
_diffrn_reflns_av_sigmaI/netI    .066
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8815
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.34
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.15
_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            pale_yellow
_exptl_crystal_density_diffrn    1.927
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             548
_exptl_crystal_size_max          .07
_exptl_crystal_size_mid          .05
_exptl_crystal_size_min          .03
_refine_diff_density_max         3.07
_refine_diff_density_min         -2.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.138
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     227
_refine_ls_number_reflns         4298
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .053
_refine_ls_R_factor_gt           .039
_refine_ls_shift/su_max          .031
_refine_ls_shift/su_mean         .002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/(sig^2(F^2) + 33F^2)
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .121
_refine_ls_wR_factor_ref         .121
_reflns_d_resolution_high        .769
_reflns_d_resolution_low         15.18
_reflns_limit_h_max              9
_reflns_limit_h_min              0
_reflns_limit_k_max              11
_reflns_limit_k_min              -11
_reflns_limit_l_max              19
_reflns_limit_l_min              -20
_reflns_number_gt                3606
_reflns_number_total             4298
_reflns_threshold_expression     'F    >  4.00 sig(F   )'
_cod_data_source_file            ic061928gsi20061205_040617_1.cif
_cod_data_source_block           cpirgn
_cod_original_sg_symbol_Hall     -p_1
_cod_database_code               4307456