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_4068643
_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_absolute_configuration syn
_chemical_formula_moiety         'C31 H36 Br N2 O2 Rh S'
_chemical_formula_sum            'C31 H36 Br N2 O2 Rh S'
_chemical_formula_weight         683.50
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.3927(4)
_cell_length_b                   16.1471(8)
_cell_length_c                   21.6575(11)
_cell_measurement_reflns_used    8103
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      29.05
_cell_measurement_theta_min      2.27
_cell_volume                     2935.0(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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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
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_diffrn_reflns_limit_h_max       11
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_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            32890
_diffrn_reflns_theta_full        29.94
_diffrn_reflns_theta_max         29.94
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    2.045
_exptl_absorpt_correction_T_max  0.850
_exptl_absorpt_correction_T_min  0.736
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.03; (Sheldrick)'
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
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_refine_diff_density_max         1.168
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_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.103(11)
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_refine_ls_number_parameters     351
_refine_ls_number_reflns         8364
_refine_ls_number_restraints     0
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_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0666P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1207
_reflns_number_gt                6923
_reflns_number_total             8364
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8009969_si_001.cif
_cod_data_source_block           rnp0602m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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      P2(1)2(1)2(1)
_cod_database_code               4068643