An amidato divalent ytterbium cluster: synthesis and molecular structure, its reactivity to carbodiimides and application in the guanylation reaction
Gong, Chao; Ding, Hao; Lu, Chengrong; Zhao, Bei; Yao, Yingming; Dalton Trans.  (2017) –; doi:10.1039/C7DT00871F

data_7042736
_publ_section_title
;
 An amidato divalent ytterbium cluster: synthesis and molecular structure,
 its reactivity to carbodiimides and application in the guanylation
 reaction
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT00871F
_journal_year                    2017
_chemical_formula_moiety         'C83 H102 N6 O4 Yb2, C61 H73 N3 O4 Yb, C7 H8'
_chemical_formula_sum            'C151 H183 N9 O8 Yb3'
_chemical_formula_weight         2771.17
_chemical_name_systematic
;
 ? 
;
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-03-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2017-03-27 deposited with the CCDC.
2017-03-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.7237(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.2664(3)
_cell_length_b                   14.09698(13)
_cell_length_c                   33.5205(4)
_cell_measurement_reflns_used    41467
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      74.2630
_cell_measurement_theta_min      3.3840
_cell_volume                     13669.5(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.3818
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_details
;
  1 omega  -94.00  -45.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0223  125.0000  150.0000 49

  2 omega  -44.00   18.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0223   38.0000    0.0000 62

  3 omega -115.00  -14.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0223  -38.0000   30.0000 101

  4 omega -121.00  -95.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.5000  -94.0000  -60.0000 26

  5 omega   53.00  118.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0391 -125.0000   60.0000 65

  6 omega   79.00  176.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0391   30.0000  142.0000 97

  7 omega  108.00  173.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0391  125.0000 -150.0000 65

  8 omega   97.00  123.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0391  125.0000 -180.0000 26

  9 omega   49.00   88.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0391  -30.0000 -150.0000 39

 10 omega   26.00   96.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0391  -94.0000  -90.0000 70

 11 omega   32.00   72.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0391  -30.0000  150.0000 40

 12 omega   74.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0391  -94.0000   30.0000 35

 13 omega   42.00   81.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0391  -45.0000  120.0000 39

 14 omega  -50.00   36.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0223   38.0000 -150.0000 86

 15 omega -114.00  -10.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0223  -57.0000  -60.0000 104

 16 omega -114.00  -10.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0223  -57.0000 -180.0000 104

 17 omega   73.00   98.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0391   77.0000 -180.0000 25

 18 omega   79.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0391   45.0000   30.0000 99

 19 omega   77.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0391   30.0000  -60.0000 101
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            92525
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.485
_diffrn_reflns_theta_min         3.055
_exptl_absorpt_coefficient_mu    4.117
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5704
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.095
_refine_diff_density_min         -1.007
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1529
_refine_ls_number_reflns         27335
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0425P)^2^+8.7536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0859
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23097
_reflns_number_total             27335
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00871f2.cif
_cod_data_source_block           g121224b
_cod_original_cell_volume        13669.5(2)
_cod_database_code               7042736
_shelx_shelxl_version_number     2014/7
_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. Restrained distances
 C14K-C14J
 1.5 with sigma of 0.02
 C135-C13B = C135-C13A
 1.58 with sigma of 0.02
3. Rigid bond restraints
 C129, C130, C131, C132, C133, C134
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C129 \\sim C130 \\sim C131 \\sim C132 \\sim C133 \\sim C134: within 1.7A with
sigma of 0.005 and sigma for terminal atoms of 0.01
Uiso(C145) = Uiso(C146) = Uiso(C147) = Uiso(C148) = Uiso(C149) = Uiso(C150) =
Uiso(C151) = Uiso(C14E) = Uiso(C14F) = Uiso(C14G) = Uiso(C14H) = Uiso(C14I) =
Uiso(C14J) = Uiso(C14K)
Uanis(C136) = Uanis(C13A)
Uanis(C137) = Uanis(C13B)
Uanis(C130) = Uanis(C131) = Uanis(C132) = Uanis(C133) = Uanis(C134) =
Uanis(C135)
5. Others
 Sof(H14A)=Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C16A)=Sof(H16D)=
 Sof(H16E)=Sof(H16F)=1-FVAR(1)
 Sof(H14)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C16)=Sof(H16A)=Sof(H16B)=
 Sof(H16C)=FVAR(1)
 Sof(H55A)=Sof(C56A)=Sof(H56D)=Sof(H56E)=Sof(H56F)=Sof(C57A)=Sof(H57D)=
 Sof(H57E)=Sof(H57F)=1-FVAR(2)
 Sof(H55)=Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=Sof(C57)=Sof(H57A)=Sof(H57B)=
 Sof(H57C)=FVAR(2)
 Sof(C13A)=Sof(H13G)=Sof(H13H)=Sof(H13I)=Sof(C13B)=Sof(H13J)=Sof(H13K)=
 Sof(H13L)=1-FVAR(3)
 Sof(C136)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C137)=Sof(H13D)=Sof(H13E)=
 Sof(H13F)=FVAR(3)
 Sof(C14A)=Sof(H14M)=Sof(H14N)=Sof(C14B)=Sof(H14O)=Sof(H14P)=Sof(C14C)=
 Sof(H14Q)=Sof(H14R)=Sof(C14D)=Sof(H14S)=Sof(H14T)=1-FVAR(4)
 Sof(C141)=Sof(H14E)=Sof(H14F)=Sof(C142)=Sof(H14G)=Sof(H14H)=Sof(C143)=
 Sof(H14I)=Sof(H14J)=Sof(C144)=Sof(H14K)=Sof(H14L)=FVAR(4)
 Sof(C14E)=Sof(H14U)=Sof(C14F)=Sof(H14V)=Sof(C14G)=Sof(H14W)=Sof(C14H)=
 Sof(H14X)=Sof(C14I)=Sof(H14Y)=Sof(C14J)=Sof(C14K)=Sof(H14Z)=Sof(H)=Sof(HA)=1-
 FVAR(5)
 Sof(C151)=Sof(H15G)=Sof(H15H)=Sof(H15I)=Sof(C145)=Sof(C146)=Sof(H146)=
 Sof(C147)=Sof(H147)=Sof(C148)=Sof(H148)=Sof(C149)=Sof(H149)=Sof(C150)=
 Sof(H150)=FVAR(5)
6.a Ternary CH refined with riding coordinates:
 C14(H14), C14(H14A), C17(H17), C33(H33), C36(H36), C52(H52), C55(H55),
 C55(H55A), C71(H71), C74(H74), C78(H78), C81(H81), C97(H97), C100(H100),
 C116(H116), C119(H119), C138(H138)
6.b Secondary CH2 refined with riding coordinates:
 C141(H14E,H14F), C142(H14G,H14H), C143(H14I,H14J), C144(H14K,H14L), C14A(H14M,
 H14N), C14B(H14O,H14P), C14C(H14Q,H14R), C14D(H14S,H14T)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12),
 C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C29(H29), C30(H30), C31(H31),
  C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C48(H48), C49(H49),
 C50(H50), C60(H60), C61(H61), C62(H62), C63(H63), C64(H64), C67(H67), C68(H68),
  C69(H69), C86(H86), C87(H87), C88(H88), C89(H89), C90(H90), C93(H93),
 C94(H94), C95(H95), C105(H105), C106(H106), C107(H107), C108(H108), C109(H109),
  C112(H112), C113(H113), C114(H114), C124(H124), C125(H125), C126(H126),
 C127(H127), C128(H128), C131(H131), C132(H132), C133(H133), C14E(H14U),
 C14F(H14V), C14G(H14W), C14H(H14X), C14I(H14Y), C146(H146), C147(H147),
 C148(H148), C149(H149), C150(H150)
6.d Fitted hexagon refined as free rotating group:
 C14E(C14F,C14G,C14H,C14I,C14J), C145(C146,C147,C148,C149,C150)
6.e Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C15A(H15D,H15E,H15F), C16A(H16D,
 H16E,H16F), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C34(H34A,H34B,H34C),
 C35(H35A,H35B,H35C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C53(H53A,H53B,
 H53C), C54(H54A,H54B,H54C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C),
 C56A(H56D,H56E,H56F), C57A(H57D,H57E,H57F), C72(H72A,H72B,H72C), C73(H73A,H73B,
 H73C), C75(H75A,H75B,H75C), C76(H76A,H76B,H76C), C79(H79A,H79B,H79C), C80(H80A,
 H80B,H80C), C82(H82A,H82B,H82C), C83(H83A,H83B,H83C), C98(H98A,H98B,H98C),
 C99(H99A,H99B,H99C), C101(H10A,H10B,H10C), C102(H10D,H10E,H10F), C117(H11A,
 H11B,H11C), C118(H11D,H11E,H11F), C120(H12A,H12B,H12C), C121(H12D,H12E,H12F),
 C136(H13A,H13B,H13C), C137(H13D,H13E,H13F), C13A(H13G,H13H,H13I), C13B(H13J,
 H13K,H13L), C139(H13M,H13N,H13O), C140(H14B,H14C,H14D), C151(H15G,H15H,H15I),
 C14K(H14Z,H,HA)
;
_olex2_submission_special_instructions 'No special instructions were received'