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_4086045
_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            'C55.5 H57 Cl2 P2 Rh'
_chemical_formula_weight         959.76
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                95.0030(10)
_cell_angle_beta                 93.9590(10)
_cell_angle_gamma                112.5340(10)
_cell_formula_units_Z            2
_cell_length_a                   11.1790(3)
_cell_length_b                   12.6005(4)
_cell_length_c                   17.9554(5)
_cell_measurement_reflns_used    9867
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.4830
_cell_measurement_theta_min      2.2915
_cell_volume                     2312.74(12)
_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-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            30742
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.511
_diffrn_reflns_theta_min         1.763
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.591
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            'clear yellow-green'
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_description       prism
_exptl_crystal_F_000             998
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.559
_refine_diff_density_min         -1.019
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.892
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         10404
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.892
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0720P)^2^+3.9411P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1012
_refine_ls_wR_factor_ref         0.1091
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8729
_reflns_number_total             10404
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00437_si_001.cif
_cod_data_source_block           hfs62_0m
_cod_depositor_comments
'Adding full bibliography for 4086045--4086050.cif.'
_cod_original_formula_sum        'C55.50 H57 Cl2 P2 Rh'
_cod_database_code               4086045
_shelx_estimated_absorpt_t_min   0.789
_shelx_estimated_absorpt_t_max   0.954
_shelxl_version_number           2014-3
_shelx_res_checksum              54820
_shelx_hkl_checksum              65417