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_7042735
_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, 3(C7 H8)'
_chemical_formula_sum            'C104 H126 N6 O4 Yb2'
_chemical_formula_weight         1870.18
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-03-27
_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                103.924(3)
_cell_angle_beta                 96.231(3)
_cell_angle_gamma                108.738(3)
_cell_formula_units_Z            2
_cell_length_a                   14.2348(4)
_cell_length_b                   16.1058(5)
_cell_length_c                   23.8596(9)
_cell_measurement_reflns_used    12226
_cell_measurement_temperature    293.01(10)
_cell_measurement_theta_max      26.1620
_cell_measurement_theta_min      3.0820
_cell_volume                     4924.1(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
'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.3818
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega   10.00   52.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -       11.0616  -99.0000 -120.0000 42

  2 omega   41.00   67.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -       11.0616  178.0000    0.0000 26

  3 omega  -25.00   28.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.4679  -99.0000  -60.0000 53

  4 omega  -83.00  -37.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.4679  -57.0000   30.0000 46

  5 omega  -36.00  -10.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.4679  -57.0000   30.0000 26

  6 omega  -97.00  -70.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.4679  178.0000   30.0000 27

  7 omega  -74.00  -31.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.4679  -37.0000  -90.0000 43

  8 omega  -83.00  -56.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.4679  147.0000  153.3613 27

  9 omega  -56.00   52.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.4679   19.0000 -180.0000 108

 10 omega  -20.00   55.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.4679   57.0000 -180.0000 75

 11 omega  -17.00   29.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.4679  -99.0000    0.0000 46
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0782
_diffrn_reflns_av_unetI/netI     0.1074
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            62644
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.793
_exptl_absorpt_coefficient_mu    1.938
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87851
_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    1.261
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.320
_refine_diff_density_min         -1.181
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     940
_refine_ls_number_reflns         20109
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.1094
_refine_ls_R_factor_gt           0.0643
_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^)+(0.0408P)^2^+20.1517P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1337
_refine_ls_wR_factor_ref         0.1486
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13505
_reflns_number_total             20109
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00871f2.cif
_cod_data_source_block           g130109a
_cod_database_code               7042735
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C91A-C97A = C91B-C97B
 1.5 with sigma of 0.02
 C84A-C90A = C84B-C90B
 1.5 with sigma of 0.02
 C98-C104 = C105-C111
 1.5 with sigma of 0.02
 C97A-C92A = C97A-C96A = C97B-C92B = C97B-C96B
 2.5 with sigma of 0.04
 C89A-C90A = C85A-C90A = C89B-C90B = C85B-C90B
 2.45 with sigma of 0.04
 C103-C104 = C99-C104 = C110-C111 = C106-C111
 2.5 with sigma of 0.04
3. Rigid bond restraints
 C71, C72, C73
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C71 \\sim C72 \\sim C73: within 1.7A with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uiso(C91A) = Uiso(C92A) = Uiso(C93A) = Uiso(C94A) = Uiso(C95A) = Uiso(C96A) =
Uiso(C97A) = Uiso(C91B) = Uiso(C92B) = Uiso(C93B) = Uiso(C94B) = Uiso(C95B) =
Uiso(C96B) = Uiso(C97B)
Uiso(C84A) = Uiso(C85A) = Uiso(C86A) = Uiso(C87A) = Uiso(C88A) = Uiso(C89A) =
Uiso(C90A) = Uiso(C84B) = Uiso(C85B) = Uiso(C86B) = Uiso(C87B) = Uiso(C88B) =
Uiso(C89B) = Uiso(C90B)
Uiso(C98) = Uiso(C99) = Uiso(C100) = Uiso(C101) = Uiso(C102) = Uiso(C103) =
Uiso(C104)
Uiso(C105) = Uiso(C106) = Uiso(C107) = Uiso(C108) = Uiso(C109) = Uiso(C110) =
Uiso(C111)
5. Others
 Fixed Sof: C84A(0.5) C85A(0.5) H85A(0.5) C86A(0.5) H86A(0.5) C87A(0.5)
 H87A(0.5) C88A(0.5) H88A(0.5) C89A(0.5) H89A(0.5) C90A(0.5) H90A(0.5)
 H90B(0.5) H90C(0.5) C84B(0.5) C85B(0.5) H85B(0.5) C86B(0.5) H86B(0.5)
 C87B(0.5) H87B(0.5) C88B(0.5) H88B(0.5) C89B(0.5) H89B(0.5) C90B(0.5)
 H90D(0.5) H90E(0.5) H90F(0.5) C91A(0.5) C92A(0.5) H92A(0.5) C93A(0.5)
 H93A(0.5) C94A(0.5) H94A(0.5) C95A(0.5) H95A(0.5) C96A(0.5) H96A(0.5)
 C97A(0.5) H97A(0.5) H97B(0.5) H97C(0.5) C91B(0.5) C92B(0.5) H92B(0.5)
 C93B(0.5) H93B(0.5) C94B(0.5) H94B(0.5) C95B(0.5) H95B(0.5) C96B(0.5)
 H96B(0.5) C97B(0.5) H97D(0.5) H97E(0.5) H97F(0.5) C98(0.5) C99(0.5) H99(0.5)
 C100(0.5) H100(0.5) C101(0.5) H101(0.5) C102(0.5) H102(0.5) C103(0.5)
 H103(0.5) C104(0.5) H10A(0.5) H10B(0.5) H10C(0.5) C105(0.5) C106(0.5)
 H106(0.5) C107(0.5) H107(0.5) C108(0.5) H108(0.5) C109(0.5) H109(0.5)
 C110(0.5) H110(0.5) C111(0.5) H11A(0.5) H11B(0.5) H11C(0.5)
6.a Ternary CH refined with riding coordinates:
 C14(H14), C17(H17), C33(H33), C36(H36), C52(H52), C55(H55), C71(H71),
 C74(H74), C78(H78), C81(H81)
6.b 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), C85A(H85A), C86A(H86A), C87A(H87A), C88A(H88A), C89A(H89A),
 C85B(H85B), C86B(H86B), C87B(H87B), C88B(H88B), C89B(H89B), C92A(H92A),
 C93A(H93A), C94A(H94A), C95A(H95A), C96A(H96A), C92B(H92B), C93B(H93B),
 C94B(H94B), C95B(H95B), C96B(H96B), C99(H99), C100(H100), C101(H101),
 C102(H102), C103(H103), C106(H106), C107(H107), C108(H108), C109(H109),
 C110(H110)
6.c Fitted hexagon refined as free rotating group:
 C84A(C85A,C86A,C87A,C88A,C89A), C84B(C85B,C86B,C87B,C88B,C89B), C91A(C92A,
 C93A,C94A,C95A,C96A), C91B(C92B,C93B,C94B,C95B,C96B), C98(C99,C100,C101,C102,
 C103), C105(C106,C107,C108,C109,C110)
6.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), 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), 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), C90A(H90A,H90B,H90C), C90B(H90D,H90E,H90F),
 C97A(H97A,H97B,H97C), C97B(H97D,H97E,H97F), C104(H10A,H10B,H10C), C111(H11A,
 H11B,H11C)
;
_olex2_submission_special_instructions 'No special instructions were received'