Investigation of the Mechanism of Alkane Reductive Elimination and Skeletal Isomerization in Tp'Rh(CNneopentyl)(R)H Complexes: The Role of Alkane Complexes
Todd O. Northcutt; Douglas D. Wick; Andrew J. Vetter; William D. Jones; Journal of the American Chemical Society 123 (2001) 7257–7270; doi:10.1021/ja003944x

data_4115625
_publ_section_title
;
 Investigation of the Mechanism of Alkane Reductive Elimination and
 Skeletal Isomerization in Tp'Rh(CNneopentyl)(R)H Complexes: The Role of
 Alkane Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7257
_journal_page_last               7270
_journal_paper_doi               10.1021/ja003944x
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C23 H38 B Cl N7 Rh'
_chemical_formula_weight         561.77
_chemical_name_common            Tp'Rh(CNneopentyl)(ethyl)Cl
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1680(15)
_cell_length_b                   15.415(3)
_cell_length_c                   16.456(3)
_cell_measurement_reflns_used    6908
_cell_measurement_temperature    193(2)
_cell_volume                     2833.0(8)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measurement_device       'Siemens SMART'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0814
_diffrn_reflns_av_sigmaI/netI    0.1020
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12164
_diffrn_reflns_theta_max         24.82
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.720
_exptl_absorpt_correction_T_max  0.927
_exptl_absorpt_correction_T_min  0.784
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            'Pale y/g'
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    NA
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.616
_refine_ls_goodness_of_fit_obs   0.594
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         4011
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.616
_refine_ls_restrained_S_obs      0.594
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_obs          0.0365
_refine_ls_shift/esd_max         -4.319
_refine_ls_shift/esd_mean        0.175
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0962
_refine_ls_wR_factor_obs         0.0843
_reflns_number_observed          3348
_reflns_number_total             4011
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja003944x_1.cif
_cod_data_source_block           sad1_jontn11
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'NA' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4115625