Surprising behaviour of M‒CO(lone pair)⋯π(arene) interactions in the solid state of fluorinated oxaphosphirane complexes
Murcia-García, Cristina; Bauzá, Antonio; Schnakenburg, Gregor; Frontera, Antonio; Streubel, Rainer; CrystEngComm 17 (2015) 1769–; doi:10.1039/C5CE00104H

data_7219337
_publ_section_title
;
 Surprising behaviour of M--CO(lone pair)&#x22EF;\p(arene) interactions in
 the solid state of fluorinated oxaphosphirane complexes
;
_journal_issue                   8
_journal_name_full               CrystEngComm
_journal_page_first              1769
_journal_paper_doi               10.1039/C5CE00104H
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C31 H19 F2 O6 P W, 0.5(C2 H2 Cl6)'
_chemical_formula_sum            'C32 H20 Cl3 F2 O6 P W'
_chemical_formula_weight         859.65
_chemical_name_systematic
; 
 ? 
;
_chemical_properties_physical    Air-sensitive
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-11-25 deposited with the CCDC.
2015-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                99.983(3)
_cell_angle_beta                 98.899(3)
_cell_angle_gamma                109.619(2)
_cell_formula_units_Z            2
_cell_length_a                   9.9709(8)
_cell_length_b                   10.8286(7)
_cell_length_c                   16.0930(15)
_cell_measurement_reflns_used    9956
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.04
_cell_measurement_theta_min      2.31
_cell_volume                     1568.9(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15563
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.64
_exptl_absorpt_coefficient_mu    4.044
_exptl_absorpt_correction_T_max  0.6879
_exptl_absorpt_correction_T_min  0.4081
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.820
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.517
_refine_diff_density_min         -1.735
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         6741
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0260
_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^)+(0.0061P)^2^+3.2268P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0524
_refine_ls_wR_factor_ref         0.0563
_reflns_number_gt                5856
_reflns_number_total             6741
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce00104h2.cif
_cod_data_source_block           2853f
_cod_depositor_comments
'Adding full bibliography for 7219337--7219339.cif.'
_cod_database_code               7219337