Dibenzo[b,f]phosphepines: Novel Phosphane‒Olefin Ligands for Transition Metals
Lyaskovskyy, Volodymyr; van Dijk-Moes, Relinde J. A.; Burck, Sebastian; Dzik, Wojciech I.; Lutz, Martin; Ehlers, Andreas W.; Slootweg, J. Chris; de Bruin, Bas; Lammertsma, Koop; Organometallics 32 (2013) 363–; doi:10.1021/om301012z

data_4079781
_publ_section_title
;
 Dibenzo[b,f]phosphepines: Novel Phosphane--Olefin Ligands for Transition
 Metals
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              363
_journal_paper_doi               10.1021/om301012z
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C60 H45 P3 Rh, C F3 O3 S'
_chemical_formula_sum            'C61 H45 F3 O3 P3 Rh S'
_chemical_formula_weight         1110.85
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.570(2)
_cell_angle_beta                 97.034(2)
_cell_angle_gamma                92.218(2)
_cell_formula_units_Z            4
_cell_length_a                   11.6114(4)
_cell_length_b                   20.7582(8)
_cell_length_c                   22.5567(9)
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.19
_cell_volume                     5254.6(3)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       Apex2
_computing_data_reduction        'SAINT V7.68A, SADABS-2008/1, Squeeze'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF-08 (Beurskens et al., 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa ApexII'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0892
_diffrn_reflns_av_sigmaI/netI    0.0960
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            83491
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    0.513
_exptl_absorpt_correction_T_max  0.4305
_exptl_absorpt_correction_T_min  0.3191
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.72
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
;
_refine_diff_density_max         2.484
_refine_diff_density_min         -1.391
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1321
_refine_ls_number_reflns         21492
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.0972
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0625P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1112
_refine_ls_wR_factor_ref         0.1227
_reflns_number_gt                13680
_reflns_number_total             21492
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om301012z_si_002.cif
_cod_data_source_block           l0386a
_cod_database_code               4079781