Platinum(0) olefin complexes of a bulky terphenylphosphine ligand. Synthetic, structural and reactivity studies
Laura Ortega-Moreno; Riccardo Peloso; Celia Maya; Andres Suarez; Ernesto Carmona; Chem.Commun. 51 (2015) 17008–; doi:10.1039/C5cc07308A

data_7118103
_publ_section_title
;
 Platinum(0) olefin complexes of a bulky terphenylphosphine ligand.
 Synthetic, structural and reactivity studies
;
_journal_name_full               Chem.Commun.
_journal_page_first              17008
_journal_paper_doi               10.1039/C5cc07308A
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C99 H129 O3 P3 Pt3'
_chemical_formula_weight         2045.20
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-07-30 deposited with the CCDC.
2015-09-25 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   18.9177(4)
_cell_length_b                   18.9177(4)
_cell_length_c                   17.4660(4)
_cell_measurement_reflns_used    9882
_cell_measurement_temperature    95(2)
_cell_measurement_theta_max      22.20
_cell_measurement_theta_min      2.50
_cell_volume                     5413.3(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      95(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_sigmaI/netI    0.0293
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            43366
_diffrn_reflns_theta_full        22.25
_diffrn_reflns_theta_max         22.25
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    2.150
_exptl_absorpt_correction_T_max  0.7447
_exptl_absorpt_correction_T_min  0.6331
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS, Bruker (2006). APEX 2. Version 2.1. Bruker Analytical
 X-ray Solutions, Madison, Wisconsin, USA. 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2052
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.931
_refine_diff_density_min         -1.222
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.644
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         4797
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.644
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+4.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0830
_reflns_number_gt                4083
_reflns_number_total             4797
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc07308a2.cif
_cod_data_source_block           4
_cod_depositor_comments
;

2018-09-03
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      P6(3)/m
_cod_original_formula_sum        'C49.50 H64.50 O1.50 P1.50 Pt1.50'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     1022.60
_cod_database_code               7118103