Selective C‒Cl Bond Oxidative Addition of Chloroarenes to a POP‒Rhodium Complex
Curto, Sheila G.; Esteruelas, Miguel A.; Oliván, Montserrat; Oñate, Enrique; Vélez, Andrea; Organometallics 36 (2017) 114–; doi:10.1021/acs.organomet.6b00615

data_4087004
_publ_section_title
;
 Selective C--Cl Bond Oxidative Addition of Chloroarenes to a POP--Rhodium
 Complex
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              114
_journal_paper_doi               10.1021/acs.organomet.6b00615
_journal_volume                  36
_journal_year                    2017
_chemical_formula_sum            'C33 H44 F O P2 Rh'
_chemical_formula_weight         640.53
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            8
_cell_length_a                   14.6602(4)
_cell_length_b                   20.0564(7)
_cell_length_c                   21.1865(8)
_cell_measurement_reflns_used    2720
_cell_measurement_temperature    150.05(10)
_cell_measurement_theta_max      25.0590
_cell_measurement_theta_min      3.5170
_cell_volume                     6229.5(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'XP, SHELXTL v. 6.14 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.14 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.3990
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.9970
_diffrn_measured_fraction_theta_max 0.8598
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_orient_matrix_UB_11      0.0012719000
_diffrn_orient_matrix_UB_12      -0.0176114000
_diffrn_orient_matrix_UB_13      0.0290005000
_diffrn_orient_matrix_UB_21      -0.0054275000
_diffrn_orient_matrix_UB_22      -0.0305635000
_diffrn_orient_matrix_UB_23      -0.0164681000
_diffrn_orient_matrix_UB_31      0.0480443000
_diffrn_orient_matrix_UB_32      -0.0029833000
_diffrn_orient_matrix_UB_33      -0.0026696000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0916
_diffrn_reflns_av_sigmaI/netI    0.1524
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            25162
_diffrn_reflns_theta_full        24.9737
_diffrn_reflns_theta_max         28.2324
_diffrn_reflns_theta_min         2.8843
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.681
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94036
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2672
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.770
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         6601
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1199
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0267P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.1084
_reflns_number_gt                3787
_reflns_number_total             6601
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00615_si_002.cif
_cod_data_source_block           17-sg125
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4087004
_cell_oxdiff_length_a            14.6651(5)
_cell_oxdiff_length_b            20.0365(17)
_cell_oxdiff_length_c            21.2005(15)
_cell_oxdiff_angle_alpha         90.026(6)
_cell_oxdiff_angle_beta          89.929(4)
_cell_oxdiff_angle_gamma         90.005(5)
_cell_oxdiff_volume              6229.5(7)
_cell_oxdiff_measurement_reflns_used 2720