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_4088098
_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         'C16 O8 Yb, 2(C29 H21)'
_chemical_formula_sum            'C74 H42 O8 Yb'
_chemical_formula_weight         1232.11
_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
_audit_creation_date             2015-09-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.70(3)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   13.268(3)
_cell_length_b                   23.619(5)
_cell_length_c                   68.846(14)
_cell_measurement_reflns_used    36013
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.999
_cell_measurement_theta_min      1.046
_cell_volume                     21530(8)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'X-Seed (Barbour, 2001)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_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  0.1092
_diffrn_reflns_av_unetI/netI     0.0657
_diffrn_reflns_Laue_measured_fraction_full 0.950
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       81
_diffrn_reflns_limit_l_min       -81
_diffrn_reflns_number            236789
_diffrn_reflns_point_group_measured_fraction_full 0.950
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.046
_diffrn_source                   'Australian Synchrotron'
_exptl_absorpt_coefficient_mu    1.351
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             7440
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
 Spek, A.L. (1990), Acta Cryst. A46, C-34
;
_refine_diff_density_max         1.937
_refine_diff_density_min         -1.953
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2242
_refine_ls_number_reflns         36013
_refine_ls_number_restraints     532
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1225
_refine_ls_R_factor_gt           0.0972
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1424P)^2^+150.7574P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2627
_refine_ls_wR_factor_ref         0.2790
_reflns_Friedel_coverage         0.000
_reflns_number_gt                26236
_reflns_number_total             36013
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00842_si_005.cif
_cod_data_source_block           7
_cod_depositor_comments
;

2020-07-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C222 H126 O24 Yb3'
_cod_original_formula_weight         3696.34
_cod_original_formula_moiety         '3(C16 O8 Yb), 6(C29 H21)'
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4088098
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C200-C201 = C200-O13 = C201-O14 = C216-C217
 1.53 with sigma of 0.02
 O17-C208 = C208-C209 = C209-O18 = O17-C207
 1.53 with sigma of 0.02
 C187-O7 = O7-C188 = C188-C189 = C189-O8 = O8-C190
 1.53 with sigma of 0.02
 C179-O3 = O3-C180 = C180-C181 = C181-O4 = O4-C182
 1.53 with sigma of 0.02
 C183-O5 = O5-C184 = C184-C185 = C185-O6 = O6-C186
 1.53 with sigma of 0.02
 O9-C191
 1.53 with sigma of 0.02
 C199-C200 = C201-C202
 2.55 with sigma of 0.02
 Yb2-C199 = Yb2-C202
 3.58 with sigma of 0.02
 Yb1-C187 = Yb1-C190 = Yb1-C178
 3.58 with sigma of 0.02
 Yb1-C179 = Yb1-C180 = Yb1-C181 = Yb1-C182
 3.58 with sigma of 0.02
 O5-O6
 2.72 with sigma of 0.02
 Yb1-C183 = Yb1-C184 = Yb1-C185 = Yb1-C186
 3.58 with sigma of 0.02
 C183-C184 = C185-C186
 2.42 with sigma of 0.02
 O17-C209 = O18-C208
 2.4 with sigma of 0.02
 Yb2-C191
 3.58 with sigma of 0.02
 C182-C183
 2.3 with sigma of 0.02
 Yb2-C201 \\sim Yb2-C200
 with sigma of 0.02
 O15-O16 \\sim O13-O14
 with sigma of 0.02
 C200-O14 \\sim C201-O13
 with sigma of 0.02
 C175-C176 \\sim C177-C178
 with sigma of 0.02
 O17-C209 \\sim O18-C208
 with sigma of 0.02
 C207-C208 \\sim C209-C210
 with sigma of 0.02
3. Rigid bond restraints
 Yb3, O17, Yb3, O18, Yb3, O19, Yb3, O20, Yb3, O21, Yb3, O22, Yb3, O23, Yb3, O24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Yb2, O9, Yb2, O10, Yb2, O11, Yb2, O12, Yb2, O13, Yb2, O14, Yb2, O15, Yb2, O16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Yb1, O1, Yb1, O2, Yb1, O3, Yb1, O4, Yb1, O5, Yb1, O6, Yb1, O7, Yb1, O8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Yb1, O5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C175 \\sim O1 \\sim C176 \\sim C177 \\sim O2 \\sim C178: within 1.7A with sigma
of 0.007 and sigma for terminal atoms of 0.001
C179 \\sim O3 \\sim C180 \\sim C181 \\sim O4 \\sim C182: within 1.7A with sigma
of 0.007 and sigma for terminal atoms of 0.001
C183 \\sim O5 \\sim C184 \\sim C185 \\sim O6 \\sim C186: within 1.7A with sigma
of 0.007 and sigma for terminal atoms of 0.001
C187 \\sim O7 \\sim C188 \\sim C189 \\sim O8 \\sim C190: within 1.7A with sigma
of 0.007 and sigma for terminal atoms of 0.001
C191 \\sim O9 \\sim C192 \\sim C193 \\sim O10 \\sim C194: within 1.7A with
sigma of 0.007 and sigma for terminal atoms of 0.001
C195 \\sim O11 \\sim C196 \\sim C197 \\sim O12 \\sim C198: within 1.7A with
sigma of 0.007 and sigma for terminal atoms of 0.001
C199 \\sim O13 \\sim C200 \\sim C201 \\sim O14 \\sim C202: within 1.7A with
sigma of 0.007 and sigma for terminal atoms of 0.001
C203 \\sim O15 \\sim C204 \\sim C205 \\sim O16 \\sim C206: within 1.7A with
sigma of 0.007 and sigma for terminal atoms of 0.001
C207 \\sim O17 \\sim C208 \\sim C209 \\sim O18 \\sim C210: within 1.7A with
sigma of 0.007 and sigma for terminal atoms of 0.001
C211 \\sim O19 \\sim C212 \\sim C213 \\sim O20 \\sim C214: within 1.7A with
sigma of 0.007 and sigma for terminal atoms of 0.001
C215 \\sim O21 \\sim C216 \\sim C217 \\sim O22 \\sim C218: within 1.7A with
sigma of 0.007 and sigma for terminal atoms of 0.001
C219 \\sim O23 \\sim C220 \\sim C221 \\sim O24 \\sim C222: within 1.7A with
sigma of 0.007 and sigma for terminal atoms of 0.001
C153 \\sim C154: within 1.7A with sigma of 0.007 and sigma for terminal atoms
of 0.001
C172 \\sim C171: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.001
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), 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), C30(H30), 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), C59(H59), C65(H65), C66(H66), C67(H67),
  C68(H68), C69(H69), C71(H71), C72(H72), C73(H73), C74(H74), C75(H75),
 C77(H77), C78(H78), C79(H79), C80(H80), C81(H81), C83(H83), C84(H84), C85(H85),
  C86(H86), C87(H87), C88(H88), C94(H94), C95(H95), C96(H96), C97(H97),
 C98(H98), C100(H100), C101(H101), C102(H102), C103(H103), C104(H104),
 C106(H106), C107(H107), C108(H108), C109(H109), C110(H110), C112(H112),
 C113(H113), C114(H114), C115(H115), C116(H116), C117(H117), C123(H123),
 C124(H124), C125(H125), C126(H126), C127(H127), C129(H129), C130(H130),
 C131(H131), C132(H132), C133(H133), C135(H135), C136(H136), C137(H137),
 C138(H138), C139(H139), C141(H141), C142(H142), C143(H143), C144(H144),
 C145(H145), C146(H146), C152(H152), C153(H153), C154(H154), C155(H155),
 C156(H156), C158(H158), C159(H159), C160(H160), C161(H161), C162(H162),
 C164(H164), C165(H165), C166(H166), C167(H167), C168(H168), C170(H170),
 C171(H171), C172(H172), C173(H173), C174(H174)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'