N–H Activation by Rh(I) via Metal–Ligand Cooperation
Feller, Moran; Diskin-Posner, Yael; Shimon, Linda J. W.; Ben-Ari, Eyal; Milstein, David; Organometallics 31 (2012) 4083–4101; doi:10.1021/om300248r

data_4078188
_publ_section_title
;
 N--H Activation by Rh(I) via Metal--Ligand Cooperation
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              4083
_journal_page_last               4101
_journal_paper_doi               10.1021/om300248r
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C25 H39 Cl2 N3 P Rh'
_chemical_formula_sum            'C25 H39 Cl2 N3 P Rh'
_chemical_formula_weight         586.37
_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                   14.1476(5)
_cell_length_b                   24.9498(9)
_cell_length_c                   7.5796(3)
_cell_measurement_reflns_used    26018
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.268
_cell_measurement_theta_min      2.6875
_cell_volume                     2675.45(17)
_computing_cell_refinement       'APEX 2'
_computing_data_collection       'APEX 2'
_computing_data_reduction        'APEX 2'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX - II kappa CCD'
_diffrn_measurement_method       'omega and phi 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  0.0518
_diffrn_reflns_av_sigmaI/netI    0.0520
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            25465
_diffrn_reflns_theta_full        28.39
_diffrn_reflns_theta_max         28.39
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    0.916
_exptl_absorpt_correction_T_max  0.9471
_exptl_absorpt_correction_T_min  0.6405
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker APEX-2'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.280
_refine_diff_density_min         -0.877
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         6691
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+2.1978P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0881
_reflns_number_gt                6136
_reflns_number_total             6691
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300248r_si_001.cif
_cod_data_source_block           complex_12
_cod_depositor_comments          'Adding value of _journal_page_last.'
_cod_original_sg_symbol_Hall     P2ac2ab
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               4078188