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_4307462
_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         'C19 H29 N4 O Rh, 2(C F3 O3 S), 3(H2 O)'
_chemical_formula_sum            'C21 H35 F6 N4 O10 Rh S2'
_chemical_formula_weight         782.54
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.00000
_cell_angle_beta                 113.902(4)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            4
_cell_length_a                   11.184(3)
_cell_length_b                   23.044(6)
_cell_length_c                   13.132(3)
_cell_measurement_reflns_used    4551
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.71
_cell_measurement_theta_min      2.18
_cell_volume                     3094.2(14)
_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(2)
_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  .045
_diffrn_reflns_av_sigmaI/netI    .064
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            28712
_diffrn_reflns_theta_full        29
_diffrn_reflns_theta_max         29
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    .779
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  .85
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS; Sheldrick, 1996
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.684
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          .24
_exptl_crystal_size_mid          .13
_exptl_crystal_size_min          .12
_refine_diff_density_max         1.042
_refine_diff_density_min         -.765
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.09
_refine_ls_goodness_of_fit_ref   1.09
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     431
_refine_ls_number_reflns         7818
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .063
_refine_ls_R_factor_gt           .043
_refine_ls_shift/su_max          .002
_refine_ls_shift/su_mean         .0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/(sig^2(F^2) +  23F^2)
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .119
_refine_ls_wR_factor_ref         .119
_reflns_d_resolution_high        .728
_reflns_d_resolution_low         11.496
_reflns_limit_h_max              15
_reflns_limit_h_min              0
_reflns_limit_k_max              30
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              -17
_reflns_number_gt                7818
_reflns_number_total             7818
_reflns_threshold_expression     'I   >  2.00 sig(I   )'
_cod_data_source_file            ic061928gsi20061205_040617_7.cif
_cod_data_source_block           cprh01
_cod_original_sg_symbol_Hall     -p_2yn
_cod_original_formula_sum        'C21 H35 F6 N4 O10 Rh1 S2'
_cod_database_code               4307462