Synthesis and energetics of Tp′Rh[P(OMe)3](R)H: a systematic investigation of ligand effects on C‒H activation at rhodium
Jiao, Yunzhe; Brennessel, William W.; Jones, William D.; Chemical Science 5 (2014) 804–; doi:10.1039/c3sc52748d

data_1513622
_publ_section_title
;
 Synthesis and energetics of Tp&#x2032;Rh[P(OMe)3](R)H: a systematic
 investigation of ligand effects on C--H activation at rhodium
;
_journal_issue                   2
_journal_name_full               'Chemical Science'
_journal_page_first              804
_journal_paper_doi               10.1039/c3sc52748d
_journal_volume                  5
_journal_year                    2014
_chemical_formula_moiety         'C19 H34 B Cl N6 O3 P Rh'
_chemical_formula_sum            'C19 H34 B Cl N6 O3 P Rh'
_chemical_formula_weight         574.66
_chemical_name_common            '3, jonyj11'
_chemical_name_systematic
; 
 ? 
;
_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'
_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                 105.977(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.0753(11)
_cell_length_b                   8.1941(5)
_cell_length_c                   33.2922(19)
_cell_measurement_reflns_used    3946
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      29.97
_cell_measurement_theta_min      2.55
_cell_volume                     5002.7(5)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD Platform'
_diffrn_measurement_method       'area detector, \w scans per \f'
_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  0.1261
_diffrn_reflns_av_sigmaI/netI    0.0846
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            138012
_diffrn_reflns_theta_full        34.97
_diffrn_reflns_theta_max         34.97
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.886
_exptl_absorpt_correction_T_max  0.9166
_exptl_absorpt_correction_T_min  0.7895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2368
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.037
_refine_diff_density_min         -1.172
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         21962
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0614
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0604P)^2^+0.6769P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1272
_refine_ls_wR_factor_ref         0.1446
_reflns_number_gt                14802
_reflns_number_total             21962
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc52748d.txt
_cod_data_source_block           3
_cod_database_code               1513622