Intramolecular C‒C Coupling Reactions of Alkynyl, Vinylidene, and Alkenylphosphane Ligands in Rhodium(III) Complexes
Martínez de Salinas, Sara; Díez, Josefina; Falvello, Larry R.; González, Javier; Gamasa, M. Pilar; Lastra, Elena; Organometallics 35 (2016) 2793–; doi:10.1021/acs.organomet.6b00330

data_4088700
_publ_section_title
;
 Intramolecular C--C Coupling Reactions of Alkynyl, Vinylidene, and
 Alkenylphosphane Ligands in Rhodium(III) Complexes
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              2793
_journal_paper_doi               10.1021/acs.organomet.6b00330
_journal_volume                  35
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C36 H47 P Rh, C F3 O3 S'
_chemical_formula_sum            'C37 H47 F3 O3 P Rh S'
_chemical_formula_weight         762.68
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0793(6)
_cell_length_b                   11.8510(5)
_cell_length_c                   32.869(2)
_cell_measurement_reflns_used    4266
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      74.3350
_cell_measurement_theta_min      3.7267
_cell_volume                     3536.7(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics    'PLATON (Spek, 2008)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    DIRDIF-2008
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 8.2640
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            9664
_diffrn_reflns_point_group_measured_fraction_full 0.879
_diffrn_reflns_point_group_measured_fraction_max 0.828
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         74.507
_diffrn_reflns_theta_min         3.965
_exptl_absorpt_coefficient_mu    5.306
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88091
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.079
_exptl_crystal_size_mid          0.033
_exptl_crystal_size_min          0.022
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details
;
 Flack x determined using 1850 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.019(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         5985
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0304
_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^)+(0.0418P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0761
_refine_ls_wR_factor_ref         0.0777
_reflns_Friedel_coverage         0.517
_reflns_Friedel_fraction_full    0.724
_reflns_Friedel_fraction_max     0.649
_reflns_number_gt                5626
_reflns_number_total             5985
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00330_si_002.cif
_cod_data_source_block           5a
_cod_database_code               4088700
_shelxl_version_number           2014-3
_shelx_res_checksum              48200
_shelx_hkl_checksum              22343