Phosphonium-based tetrakis dibenzoylmethane Eu(III) and Sm(III) complexes: synthesis, crystal structure and photoluminescence properties in a weakly coordinating phosphonium ionic liquid
Malba, Chandrashekhar Marotirao; Enrichi, Francesco; Facchin, Manuela; Demitri, Nicola; Plaisier, Jasper Rikkert; Natile, Marta Maria; Selva, Maurizio; Riello, Pietro; Perosa, Alvise; Benedetti, A.; RSC Adv.  (2015) –; doi:10.1039/C5RA03947A

data_7221003
_publ_section_title
;
 Phosphonium-based tetrakis dibenzoylmethane Eu(III) and Sm(III)
 complexes: synthesis, crystal structure and photoluminescence properties
 in a weakly coordinating phosphonium ionic liquid
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA03947A
_journal_year                    2015
_chemical_formula_moiety         'C60 H44 O8 Sm, C25 H54 P'
_chemical_formula_sum            'C85 H98 O8 P Sm'
_chemical_formula_weight         1428.95
_chemical_name_common            '[P8,8,8,1][Sm(dbm)4]'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-03-03 deposited with the CCDC.
2015-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.60(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.169(3)
_cell_length_b                   22.341(4)
_cell_length_c                   20.962(2)
_cell_measurement_reflns_used    10667
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.253
_cell_measurement_theta_min      1.176
_cell_volume                     7443(2)
_computing_cell_refinement       XDS
_computing_data_collection       'Elettra XRD1 Data Collection SW'
_computing_data_reduction        'XDS - CCP4'
_computing_molecular_graphics    'Ortep3 for Windows'
_computing_publication_material  enCIFer/publCIF
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    Sir2011
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type
;
'Huber 4-circles Kappa Goniometer, Pilatus 2M detector'
;
_diffrn_measurement_method       'Rotating crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6525
_diffrn_reflns_av_unetI/netI     0.0606
_diffrn_reflns_laue_measured_fraction_full 0.966
_diffrn_reflns_laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10324
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        21.253
_diffrn_reflns_theta_max         21.253
_diffrn_reflns_theta_min         1.176
_diffrn_source                   'Elettra Synchrotron - XRD1 BL'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.638
_exptl_absorpt_correction_T_max  2.226
_exptl_absorpt_correction_T_min  0.250
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
        Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56
        Cubic fit to sin(theta)/lambda - 24 parameters
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       'Thin needles'
_exptl_crystal_F_000             2996
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         3.054
_refine_diff_density_min         -1.349
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     763
_refine_ls_number_reflns         10324
_refine_ls_number_restraints     1055
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1197
_refine_ls_R_factor_gt           0.0879
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1298P)^2^+39.5078P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2248
_refine_ls_wR_factor_ref         0.2559
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7707
_reflns_number_total             10324
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra03947a2.cif
_cod_data_source_block           Smdbm4P
_cod_database_code               7221003
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.883
_shelx_estimated_absorpt_t_max   0.969