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_4079782
_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         'C46 H42 P2 Rh, C F3 O3 S, 1.5(C H2 Cl2)'
_chemical_formula_sum            'C48.5 H45 Cl3 F3 O3 P2 Rh S'
_chemical_formula_weight         1036.10
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.9135(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.2103(5)
_cell_length_b                   23.0846(9)
_cell_length_c                   16.4554(6)
_cell_measurement_reflns_used    9273
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.64
_cell_measurement_theta_min      2.56
_cell_volume                     4482.0(3)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       Apex
_computing_data_reduction        'SAINT V7.68A, Sadabs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0175
_diffrn_reflns_av_sigmaI/netI    0.0120
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            54153
_diffrn_reflns_theta_full        27.67
_diffrn_reflns_theta_max         27.67
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    0.733
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6412
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2116
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.939
_refine_diff_density_min         -0.791
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         10385
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.237
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0284
_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^)+(0.0292P)^2^+5.0427P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0725
_reflns_number_gt                9525
_reflns_number_total             10385
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om301012z_si_002.cif
_cod_data_source_block           l0108a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C48.50 H45 Cl3 F3 O3 P2 Rh S'
_cod_database_code               4079782