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_4079780
_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         'C68 H86 Na4 O7 P2'
_chemical_formula_sum            'C68 H86 Na4 O7 P2'
_chemical_formula_weight         1169.27
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 92.312(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.616(2)
_cell_length_b                   10.2843(5)
_cell_length_c                   21.7045(13)
_cell_measurement_reflns_used    32567
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.66
_cell_volume                     6828.4(7)
_computing_cell_refinement       Peakref
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'Eval15, 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 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0244
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            46590
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    0.137
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6911
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.27
_platon_squeeze_details
;
;
_refine_diff_density_max         0.802
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         7680
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0702P)^2^+4.9718P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1295
_refine_ls_wR_factor_ref         0.1384
_reflns_number_gt                5894
_reflns_number_total             7680
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om301012z_si_002.cif
_cod_data_source_block           s4331a
_cod_original_cell_volume        6828.5(7)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4079780