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_7120173
_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            'C38 H50 N P2 Rh Zn'
_chemical_formula_weight         751.01
_chemical_name_systematic        (PNP)Rh(ZnPh)(Ph)
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-03-11 deposited with the CCDC.
2017-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.766(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.751(2)
_cell_length_b                   37.418(7)
_cell_length_c                   17.055(4)
_cell_measurement_reflns_used    9713
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      55.422
_cell_measurement_theta_min      4.921
_cell_volume                     7057(2)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0222
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            41364
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.708
_diffrn_reflns_theta_min         2.177
_exptl_absorpt_coefficient_mu    1.265
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6341
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_description       block
_exptl_crystal_F_000             3120
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pentane'
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.602
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Flack x determined using 7591 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.036(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     796
_refine_ls_number_reflns         16168
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0225
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0217P)^2^+5.0036P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0536
_refine_ls_wR_factor_ref         0.0542
_reflns_Friedel_coverage         0.993
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.986
_reflns_number_gt                15930
_reflns_number_total             16168
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc02707a2.cif
_cod_data_source_block           oz565_cjp1009
_cod_database_code               7120173
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.751
_shelx_estimated_absorpt_t_max   0.873
_shelx_res_checksum              20501