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_4088528
_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 H46 Cl P2 Rh'
_chemical_formula_sum            'C29 H46 Cl P2 Rh'
_chemical_formula_weight         594.96
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.469
_cell_length_b                   12.732
_cell_length_c                   15.832
_cell_measurement_reflns_used    9000
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      66.71
_cell_measurement_theta_min      4.30
_cell_volume                     3521.279
_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.  5.1.0'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.995
_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  0.0273
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22341
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.780
_diffrn_reflns_theta_min         3.471
_exptl_absorpt_coefficient_mu    5.559
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6175
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;

;
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.041(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         5345
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0241
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+0.6938P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0611
_refine_ls_wR_factor_ref         0.0614
_reflns_Friedel_coverage         0.921
_reflns_Friedel_fraction_full    0.976
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                5206
_reflns_number_total             5345
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00155_si_002.cif
_cod_data_source_block           4_Cl_trans
_cod_original_cell_volume        3521.3
_cod_database_code               4088528
_shelxl_version_number           2013-4
_shelx_res_checksum              19175
_shelx_hkl_checksum              19740