Divalent Tetra- and Penta-phenylcyclopentadienyl Europium and Samarium Sandwich and Half-Sandwich Complexes: Synthesis, Characterization, and Remarkable Luminescence Properties
Kelly, Rory P.; Bell, Toby D. M.; Cox, Rosalind P.; Daniels, Daisy P.; Deacon, Glen B.; Jaroschik, Florian; Junk, Peter C.; Le Goff, Xavier F.; Lemercier, Gilles; Martinez, Agathe; Wang, Jun; Werner, Daniel; Organometallics 34 (2015) 5624–; doi:10.1021/acs.organomet.5b00842

data_4088099
_publ_section_title
;
 Divalent Tetra- and Penta-phenylcyclopentadienyl Europium and Samarium
 Sandwich and Half-Sandwich Complexes: Synthesis, Characterization, and
 Remarkable Luminescence Properties
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              5624
_journal_paper_doi               10.1021/acs.organomet.5b00842
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C70 H50 Eu'
_chemical_formula_sum            'C70 H50 Eu'
_chemical_formula_weight         1043.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-08-11
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.39(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.425(2)
_cell_length_b                   13.463(3)
_cell_length_c                   18.070(4)
_cell_measurement_reflns_used    16868
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.498
_cell_measurement_theta_min      2.172
_cell_volume                     2524.9(9)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_reflns_av_R_equivalents  0.0568
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16868
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.498
_diffrn_reflns_theta_max         25.498
_diffrn_reflns_theta_min         2.172
_diffrn_source                   'Australian Synchrotron'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.286
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             1066
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.374
_refine_diff_density_min         -1.695
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         4689
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0526
_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^)+(0.0606P)^2^+3.6569P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1243
_refine_ls_wR_factor_ref         0.1383
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3480
_reflns_number_total             4689
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00842_si_001.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4088099
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C25(H25), C29(H29), C28(H28), C8(H8), C31(H31), C35(H35), C32(H32),
 C11(H11), C33(H33), C26(H26), C23(H23), C34(H34), C27(H27), C9(H9), C19(H19),
 C13(H13), C10(H10), C16(H16), C14(H14), C17(H17), C22(H22), C15(H15), C21(H21),
  C20(H20)
;
_shelx_res_checksum              84163
_shelx_hkl_checksum              63368
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'