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_4088526
_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         'C50 H76 Cl2 P4 Rh2'
_chemical_formula_sum            'C50 H76 Cl2 P4 Rh2'
_chemical_formula_weight         1077.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 93.648(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.2923(5)
_cell_length_b                   15.5647(5)
_cell_length_c                   17.7431(4)
_cell_measurement_reflns_used    8100
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.1
_cell_measurement_theta_min      0.998
_cell_volume                     5317.1(3)
_computing_cell_refinement       'DENZO & ScalePACK (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'Denzo and ScalePACK'
_computing_molecular_graphics    'SHELXTL (Bruker, 2013)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Nonius Kappa CCD area detector'
_diffrn_measurement_method       '\w & \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16153
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.647
_diffrn_source                   'Fine focused sealed X-Ray tube'
_exptl_absorpt_coefficient_mu    0.873
_exptl_absorpt_correction_T_max  0.820
_exptl_absorpt_correction_T_min  0.732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ScalePACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_description       block
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.220
_platon_squeeze_details
; The heavily disordered guest molecules were squeezed out 
by using the sub-routine "SQUEEZE" in Platon.
;
_refine_diff_density_max         1.313
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.205
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         10188
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.219
_refine_ls_R_factor_all          0.1026
_refine_ls_R_factor_gt           0.0813
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0431P)^2^+56.0896P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1838
_refine_ls_wR_factor_ref         0.1989
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8345
_reflns_number_total             10188
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00155_si_002.cif
_cod_data_source_block           1_trans
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4088526
_shelx_estimated_absorpt_t_min   0.733
_shelx_estimated_absorpt_t_max   0.831
_shelxl_version_number           2014/6
_shelx_res_checksum              91981
_shelx_hkl_checksum              98966