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_4088701
_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_formula_moiety         'C35 H45 P Rh 1+, B F4 1-'
_chemical_formula_sum            'C35 H45 B F4 P Rh'
_chemical_formula_weight         686.40
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P -2ac -2n'
_space_group_name_H-M_alt        'P n 21 a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/8
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.4176(2)
_cell_length_b                   33.1623(4)
_cell_length_c                   9.16578(11)
_cell_measurement_reflns_used    13137
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      69.542
_cell_measurement_theta_min      4.114
_cell_volume                     6510.06(13)
_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
;
PLATON (Spek, 2008)
Diamond Version 3.2k (Crystal Impact, 2014)
;
_computing_publication_material  'WinGX publication routines (Farrugia, 2012'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    DIRDIF-2008
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.2640
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            28988
_diffrn_reflns_point_group_measured_fraction_full 0.958
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         69.672
_diffrn_reflns_theta_min         4.128
_diffrn_source                   'Nova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.086
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58112
_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)
Multi-scan absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_description       prism
_exptl_crystal_F_000             2848
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.544
_refine_diff_density_min         -0.780
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
;
 Flack x determined using 4218 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.032(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1220
_refine_ls_number_reflns         11492
_refine_ls_number_restraints     1150
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0856P)^2^+3.8235P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1371
_reflns_Friedel_coverage         0.866
_reflns_Friedel_fraction_full    0.914
_reflns_Friedel_fraction_max     0.886
_reflns_number_gt                10332
_reflns_number_total             11492
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00330_si_002.cif
_cod_data_source_block           11a
_cod_database_code               4088701
_shelx_shelxl_version_number     2014/8
_shelx_estimated_absorpt_t_min   0.320
_shelx_estimated_absorpt_t_max   0.785
_shelx_res_checksum              89303
_shelx_hkl_checksum              5520