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_4088097
_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         'C41 H45 I O3 Sm, C4 H8 O'
_chemical_formula_sum            'C45 H53 I O4 Sm'
_chemical_formula_weight         935.12
_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     direct
_audit_creation_date             2015-08-14
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 104.45(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.583(4)
_cell_length_b                   10.701(2)
_cell_length_c                   17.660(4)
_cell_measurement_reflns_used    67218
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.773
_cell_measurement_theta_min      0.974
_cell_volume                     3949.7(15)
_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 0.955
_diffrn_measured_fraction_theta_max 0.907
_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     0.7107
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_full 0.955
_diffrn_reflns_Laue_measured_fraction_max 0.907
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            67218
_diffrn_reflns_point_group_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.907
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         28.773
_diffrn_reflns_theta_min         0.974
_diffrn_source                   'Australian Synchrotron'
_exptl_absorpt_coefficient_mu    2.310
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.227
_refine_diff_density_min         -1.826
_refine_diff_density_rms         0.136
_refine_ls_extinction_coef       0.00633(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         9322
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+10.0138P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0842
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8316
_reflns_number_total             9322
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00842_si_006.cif
_cod_data_source_block           8
_cod_original_cell_volume        3949.7(14)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4088097
_shelx_estimated_absorpt_t_max   0.955
_shelx_estimated_absorpt_t_min   0.769
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O4-C42 = O4-C45
 1.45 with sigma of 0.01
 C42-C43 = C44-C45
 1.51 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C38(H38A,H38B), C32(H32A,H32B), C30(H30A,H30B), C33(H33A,H33B), C39(H39A,
 H39B), C40(H40A,H40B), C41(H41A,H41B), C37(H37A,H37B), C31(H31A,H31B),
 C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C45(H45A,H45B), C43(H43A,H43B),
  C44(H44A,H44B), C42(H42A,H42B)
3.b Aromatic/amide H refined with riding coordinates:
 C29(H29), C27(H27), C9(H9), C13(H13), C20(H20), C8(H8), C17(H17), C23(H23),
 C22(H22), C1(H1), C28(H28), C11(H11), C19(H19), C10(H10), C25(H25), C7(H7),
 C21(H21), C26(H26), C14(H14), C16(H16), C15(H15)
;
_shelx_res_checksum              50285
_shelx_hkl_checksum              16598
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'