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_1513621
_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         'C18 H31 B Cl2 N6 O3 P Rh'
_chemical_formula_sum            'C18 H31 B Cl2 N6 O3 P Rh'
_chemical_formula_weight         595.08
_chemical_name_common            '1, jonyj09'
_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                 90.104(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.677(3)
_cell_length_b                   12.392(3)
_cell_length_c                   18.636(4)
_cell_measurement_reflns_used    3912
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      37.71
_cell_measurement_theta_min      2.20
_cell_volume                     2465.7(11)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL (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 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0667
_diffrn_reflns_av_sigmaI/netI    0.0526
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            73278
_diffrn_reflns_theta_full        37.78
_diffrn_reflns_theta_max         37.78
_diffrn_reflns_theta_min         1.09
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.006
_exptl_absorpt_correction_T_max  0.9238
_exptl_absorpt_correction_T_min  0.7389
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.279
_refine_diff_density_min         -1.653
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         13043
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0312P)^2^+2.1710P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0894
_reflns_number_gt                10760
_reflns_number_total             13043
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc52748d.txt
_cod_data_source_block           1
_cod_original_cell_volume        2465.8(10)
_cod_database_code               1513621