κ3(P,C,C)-Allylphosphane Iridium(III) and Rhodium(III) Complexes: Preparation and Reactivity toward Nucleophilic Reagents
Sánchez-Sordo, Irene; Salinas, Sara Mart\?ínez de; D\?íez, Josefina; Lastra, Elena; Gamasa, M. Pilar; Organometallics 34 (2015) 4581–; doi:10.1021/acs.organomet.5b00665

data_4086259
_publ_section_title
;
 \k3(P,C,C)-Allylphosphane Iridium(III) and Rhodium(III) Complexes:
 Preparation and Reactivity toward Nucleophilic Reagents
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4581
_journal_paper_doi               10.1021/acs.organomet.5b00665
_journal_volume                  34
_journal_year                    2015
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C32 H47 Cl Ir P2, C24 H20 B, C H2 Cl2'
_chemical_formula_sum            'C57 H69 B Cl3 Ir P2'
_chemical_formula_weight         1125.42
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                97.749(2)
_cell_angle_beta                 99.170(2)
_cell_angle_gamma                111.495(2)
_cell_formula_units_Z            2
_cell_length_a                   13.7203(17)
_cell_length_b                   14.2700(17)
_cell_length_c                   15.7110(19)
_cell_measurement_reflns_used    9488
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.89
_cell_measurement_theta_min      2.24
_cell_volume                     2762.3(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            47108
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.987
_diffrn_reflns_theta_min         2.241
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.654
_exptl_absorpt_correction_T_max  0.3340
_exptl_absorpt_correction_T_min  0.2220
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v.2008/1;(Sheldrick 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1148
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;

;
_refine_diff_density_max         6.432
_refine_diff_density_min         -3.340
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         13142
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0451
_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^)+(0.0712P)^2^+7.1400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1180
_refine_ls_wR_factor_ref         0.1230
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11353
_reflns_number_total             13142
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00665_si_002.cif
_cod_data_source_block           6
_cod_database_code               4086259
_shelxl_version_number           2014-3
_shelx_res_checksum              136
_shelx_hkl_checksum              8776