Formation of (PNP)Rh complexes containing covalent rhodium-zinc bonds in studies of potential Rh-catalysed Negishi coupling
Pell, Christopher J.; Shih, Wei-Chun; Gatard, Sylvain; Ozerov, Oleg V.; Chem. Commun.  (2017) –; doi:10.1039/C7CC02707A

data_7120175
_publ_section_title
;
 Formation of (PNP)Rh complexes containing covalent rhodium-zinc bonds in
 studies of potential Rh-catalysed Negishi coupling
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC02707A
_journal_year                    2017
_chemical_formula_sum            'C57 H92 Cl4 N2 P4 Rh2 Zn'
_chemical_formula_weight         1342.19
_chemical_name_systematic        '[(PNP)Rh(H)]2[?-ZnCl4]'
_chemical_properties_physical    ', Air-sensitive'
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-03-11 deposited with the CCDC.
2017-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.463(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5314(3)
_cell_length_b                   26.3935(7)
_cell_length_c                   23.9279(8)
_cell_measurement_reflns_used    9990
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      116.080
_cell_measurement_theta_min      4.987
_cell_volume                     6644.9(3)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.952
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            64176
_diffrn_reflns_point_group_measured_fraction_full 0.952
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        58.202
_diffrn_reflns_theta_max         58.202
_diffrn_reflns_theta_min         2.494
_exptl_absorpt_coefficient_mu    7.037
_exptl_absorpt_correction_T_max  0.7514
_exptl_absorpt_correction_T_min  0.6035
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_description       block
_exptl_crystal_F_000             2784
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Diethyl ether, pentane'
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.942
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         8887
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0393P)^2^+36.4091P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1137
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7444
_reflns_number_total             8887
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc02707a2.cif
_cod_data_source_block           cjp1126
_cod_database_code               7120175
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              97207
_shelx_fab_checksum              10949