Reactivity, Structures, and NMR Spectroscopy of Half-Sandwich Pentamethylcyclopentadienyl Rhodium Amido Complexes Relevant to Transfer Hydrogenation
Blacker, A. John; Duckett, Simon B.; Grace, Jake; Perutz, Robin N.; Whitwood, Adrian C.; Organometallics 28 (2009) 1435–; doi:10.1021/om8009969

data_4068644
_publ_section_title
;
 Reactivity, Structures, and NMR Spectroscopy of Half-Sandwich
 Pentamethylcyclopentadienyl Rhodium Amido Complexes Relevant to Transfer
 Hydrogenation
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1435
_journal_paper_doi               10.1021/om8009969
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C21 H32 Cl O2 Rh2, C24 H20 B, C4 H10 O'
_chemical_formula_sum            'C49 H62 B Cl O3 Rh2'
_chemical_formula_weight         951.07
_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_method           SHELXL-97
_cell_angle_alpha                106.264(2)
_cell_angle_beta                 92.571(2)
_cell_angle_gamma                92.506(2)
_cell_formula_units_Z            2
_cell_length_a                   11.7528(10)
_cell_length_b                   13.6373(12)
_cell_length_c                   14.2877(12)
_cell_measurement_reflns_used    9546
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.26
_cell_volume                     2192.3(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22323
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    0.854
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.650
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.03; (Sheldrick)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.351
_refine_diff_density_min         -0.983
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         10753
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0398P)^2^+2.4272P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0889
_reflns_number_gt                9115
_reflns_number_total             10753
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8009969_si_001.cif
_cod_data_source_block           rnp0608m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4068644