Different Coordination Modes of the Ph2PCsp3PPh2Pincer Ligand in Rhodium Complexes as a Consequence of Csp3‒H Metal Interaction
Arras, Janet; Speth, Hansjörg; Mayer, Hermann A.; Wesemann, Lars; Organometallics 34 (2015) 3629–; doi:10.1021/acs.organomet.5b00437

data_4086048
_publ_section_title
;
 Different Coordination Modes of the Ph2PCsp3PPh2Pincer Ligand in Rhodium
 Complexes as a Consequence of Csp3--H Metal Interaction
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3629
_journal_paper_doi               10.1021/acs.organomet.5b00437
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C76 H76 Cl N P3 Rh'
_chemical_formula_weight         1234.65
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.4850(5)
_cell_length_b                   14.6044(2)
_cell_length_c                   13.3357(2)
_cell_measurement_reflns_used    318
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      26.6349
_cell_measurement_theta_min      2.8533
_cell_volume                     6326.78(16)
_computing_cell_refinement       'APEX2 v2011.8-0 (Bruker AXS)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_sigmaI/netI    0.0760
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            75679
_diffrn_reflns_theta_full        29.98
_diffrn_reflns_theta_max         29.98
_diffrn_reflns_theta_min         1.88
_diffrn_source_type              'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.432
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2584
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.672
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.014(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     794
_refine_ls_number_reflns         18149
_refine_ls_number_restraints     141
_refine_ls_restrained_S_all      0.943
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0280P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0721
_reflns_number_gt                14538
_reflns_number_total             18149
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00437_si_001.cif
_cod_data_source_block           compound5_JA20_0m
_cod_depositor_comments
'Adding full bibliography for 4086045--4086050.cif.'
_cod_database_code               4086048