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_4088101
_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         'C62 H52 Eu O2, 1.5(C4 H10 O2)'
_chemical_formula_sum            'C68 H67 Eu O5'
_chemical_formula_weight         1116.17
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2015-08-10
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.081(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.2090(6)
_cell_length_b                   20.0023(11)
_cell_length_c                   44.869(3)
_cell_measurement_reflns_used    116013
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.314
_cell_measurement_theta_min      1.712
_cell_volume                     10873.8(11)
_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 (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_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     0.712
_diffrn_reflns_av_R_equivalents  0.0638
_diffrn_reflns_av_unetI/netI     0.0782
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -63
_diffrn_reflns_number            116013
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.314
_diffrn_reflns_theta_min         1.712
_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    1.206
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4624
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.989
_refine_diff_density_min         -0.968
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1343
_refine_ls_number_reflns         32305
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0537
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0148P)^2^+23.2040P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.1004
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20386
_reflns_number_total             32305
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00842_si_004.cif
_cod_data_source_block           5
_cod_original_cell_volume        10873.8(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4088101
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C60(H60A,H60B), C61(H61A,H61B), C122(H12D,H12E), C123(H12F,H12G), C126(H12N,
 H12O), C127(H12P,H12Q), C130(H13A,H13B), C131(H13C,H13D), C134(H13K,H13L),
 C135(H13M,H13N)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C30(H30), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13),
 C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22),
  C23(H23), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C36(H36),
 C37(H37), C38(H38), C39(H39), C40(H40), C42(H42), C43(H43), C44(H44), C45(H45),
  C46(H46), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C54(H54),
 C55(H55), C56(H56), C57(H57), C58(H58), C63(H63), C69(H69), C70(H70), C71(H71),
  C72(H72), C73(H73), C75(H75), C76(H76), C77(H77), C78(H78), C79(H79),
 C81(H81), C82(H82), C83(H83), C84(H84), C85(H85), C87(H87), C88(H88), C89(H89),
  C90(H90), C91(H91), C92(H92), C98(H98), C99(H99), C100(H100), C101(H101),
 C102(H102), C104(H104), C105(H105), C106(H106), C107(H107), C108(H108),
 C110(H110), C111(H111), C112(H112), C113(H113), C114(H114), C116(H116),
 C117(H117), C118(H118), C119(H119), C120(H120)
2.c Idealised Me refined as rotating group:
 C59(H59A,H59B,H59C), C62(H62A,H62B,H62C), C121(H12A,H12B,H12C), C124(H12H,
 H12I,H12J), C125(H12K,H12L,H12M), C128(H12R,H12S,H12T), C129(H12U,H12V,H12W),
 C132(H13E,H13F,H13G), C133(H13H,H13I,H13J), C136(H13O,H13P,H13Q)
;
_shelx_res_checksum              29745
_shelx_hkl_checksum              24533
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'