Ligand Attachment Chemistry in the Preparation of PCsp3P and PCsp2P Complexes of Rhodium
Logan, Jessamyn R.; Piers, Warren E.; Borau-Garcia, Javier; Spasyuk, Denis M.; Organometallics 35 (2016) 1279–; doi:10.1021/acs.organomet.6b00155

data_4088530
_publ_section_title
;
 Ligand Attachment Chemistry in the Preparation of PCsp3P and PCsp2P
 Complexes of Rhodium
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              1279
_journal_paper_doi               10.1021/acs.organomet.6b00155
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C29 H44 Cl P2 Rh'
_chemical_formula_sum            'C29 H44 Cl P2 Rh'
_chemical_formula_weight         592.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 96.735(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.571(3)
_cell_length_b                   22.777(7)
_cell_length_c                   14.932(4)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      66.69
_cell_measurement_theta_min      3.56
_cell_volume                     2894.9(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'LinXTL v.  5.1.2'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18971
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         66.757
_diffrn_reflns_theta_min         3.557
_exptl_absorpt_coefficient_mu    6.762
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.4943
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.569
_refine_diff_density_min         -1.662
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         5090
_refine_ls_number_restraints     313
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0369
_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^)+(0.0415P)^2^+6.9325P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0908
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4851
_reflns_number_total             5090
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00155_si_002.cif
_cod_data_source_block           5-Cl
_cod_original_cell_volume        2894.9(14)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4088530
_shelxl_version_number           2013-4
_shelx_res_checksum              12981
_shelx_hkl_checksum              53519