Di and trinuclear rare-earth metal complexes supported by 3-amido appended indolyl ligands: synthesis, characterization and catalytic activity towards isoprene 1,4-cis polymerization.
Zhang, Guangchao; Deng, Baojia; Wang, Shaowu; Wei, Yun; Zhou, Shuangliu; Zhu, Xiancui; Huang, Zeming; Mu, Xiaolong; Dalton transactions (Cambridge, England : 2003) 45 (2016) 15445–; doi:10.1039/c6dt02922a

data_7040449
_publ_section_title
;
 Di and trinuclear rare-earth metal complexes supported by 3-amido
 appended indolyl ligands: synthesis, characterization and catalytic
 activity towards isoprene 1,4-cis polymerization.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15445
_journal_paper_doi               10.1039/c6dt02922a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C60 H102 N6 O4 Si4 Y2'
_chemical_formula_sum            'C60 H102 N6 O4 Si4 Y2'
_chemical_formula_weight         1261.66
_chemical_name_systematic
;
 ? 
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-10-30
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.08.17 svn.r3210 for OlexSys, GUI svn.r5083)
;
_audit_update_record
;
2016-04-25 deposited with the CCDC.
2016-08-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.655(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.873(3)
_cell_length_b                   15.102(2)
_cell_length_c                   30.748(5)
_cell_measurement_reflns_used    9732
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.60
_cell_measurement_theta_min      2.26
_cell_volume                     7063(2)
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD Area Detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1780
_diffrn_reflns_av_unetI/netI     0.1232
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            52781
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         1.499
_exptl_absorpt_coefficient_mu    1.747
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2680
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.261
_refine_diff_density_min         -0.984
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     805
_refine_ls_number_reflns         13377
_refine_ls_number_restraints     297
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1542
_refine_ls_R_factor_gt           0.0830
_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^)+(0.0823P)^2^+24.3504P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1881
_refine_ls_wR_factor_ref         0.2340
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7711
_reflns_number_total             13377
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02922a2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7040444--7040455.cif.'
_cod_database_code               7040449
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1-C2
 1.5 with sigma of 0.02
 C1A-C2A
 1.5 with sigma of 0.02
 C3AA-C4AA \\sim C3-C4
 with sigma of 0.02
 C3-C2AA \\sim C2AA-C3AA
 with sigma of 0.02
 C4-C1AA \\sim C1AA-C4AA
 with sigma of 0.02
 C2A-C35 \\sim C35-C2
 with sigma of 0.02
 C1-C19A \\sim C19A-C1A
 with sigma of 0.02
 C1-C2 \\sim C1A-C2A
 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(C2A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C1) \\sim Ueq, Uanis(C1A) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.01
5. Others
 Sof(H05C)=Sof(H05D)=Sof(C06A)=Sof(H06C)=Sof(H06D)=Sof(C3B)=Sof(H3BA)=
 Sof(H3BB)=Sof(C6A)=Sof(H6A)=1-FVAR(1)
 Sof(C6B)=Sof(H6B)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H05A)=Sof(H05B)=Sof(C06)=
 Sof(H06A)=Sof(H06B)=FVAR(1)
 Sof(H40C)=Sof(H40D)=Sof(H12C)=Sof(H12D)=Sof(C2X)=Sof(H2XA)=Sof(H2XB)=Sof(C1F)=
 Sof(H1FA)=Sof(H1FB)=1-FVAR(2)
 Sof(H40A)=Sof(H40B)=Sof(H12A)=Sof(H12B)=Sof(C1E)=Sof(H1EA)=Sof(H1EB)=Sof(C2W)=
 Sof(H2WA)=Sof(H2WB)=FVAR(2)
 Sof(C09A)=Sof(H09D)=Sof(H09E)=Sof(H09F)=1-FVAR(3)
 Sof(C09)=Sof(H09A)=Sof(H09B)=Sof(H09C)=FVAR(3)
 Sof(C04A)=Sof(H04D)=Sof(H04E)=Sof(H04F)=1-FVAR(4)
 Sof(C04)=Sof(H04A)=Sof(H04B)=Sof(H04C)=FVAR(4)
 Sof(H16C)=Sof(H16D)=1-FVAR(5)
 Sof(H16A)=Sof(H16B)=FVAR(5)
 Sof(H1AC)=Sof(H1AD)=Sof(H2AC)=Sof(H2AD)=Sof(C3AA)=Sof(H3AC)=Sof(H3AD)=
 Sof(C4AA)=Sof(H4AC)=Sof(H4AD)=1-FVAR(6)
 Sof(H1AA)=Sof(H1AB)=Sof(H2AA)=Sof(H2AB)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C4)=
 Sof(H4A)=Sof(H4B)=FVAR(6)
 Sof(H35C)=Sof(H35D)=Sof(H19C)=Sof(H19D)=Sof(C2A)=Sof(H2AE)=Sof(H2AF)=Sof(C1A)=
 Sof(H1AE)=Sof(H1AF)=1-FVAR(7)
 Sof(H35A)=Sof(H35B)=Sof(H19A)=Sof(H19B)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=
 Sof(H2A)=Sof(H2B)=FVAR(7)
6.a Ternary CH refined with riding coordinates:
 C14(H14), C16(H16), C20(H20), C6B(H6B), C6A(H6A)
6.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C29(H29A,H29B), C30(H30A,H30B), C22(H22A,H22B), C40(H40A,
 H40B), C40(H40C,H40D), C35(H35A,H35B), C35(H35C,H35D), C0(H0A,H0B), C19A(H19A,
 H19B), C19A(H19C,H19D), C18A(H18A,H18B), C17A(H17A,H17B), C16A(H16A,H16B),
 C16A(H16C,H16D), C15A(H15A,H15B), C12H(H12A,H12B), C12H(H12C,H12D), C11A(H11A,
 H11B), C4A(H4AA,H4AB), C3A(H3AA,H3AB), C1E(H1EA,H1EB), C05(H05A,H05B),
 C05(H05C,H05D), C2W(H2WA,H2WB), C06(H06A,H06B), C06A(H06C,H06D), C3B(H3BA,
 H3BB), C2X(H2XA,H2XB), C1F(H1FA,H1FB), C1AA(H1AA,H1AB), C1AA(H1AC,H1AD),
 C2AA(H2AA,H2AB), C2AA(H2AC,H2AD), C3(H3A,H3B), C4(H4A,H4B), C1(H1A,H1B),
 C2(H2A,H2B), C3AA(H3AC,H3AD), C4AA(H4AC,H4AD), C2A(H2AE,H2AF), C1A(H1AE,H1AF)
6.c Aromatic/amide H refined with riding coordinates:
 C0AA(H0AA), C17(H17), C41(H41), C27(H27), C25(H25), C31(H31), C34(H34),
 C32(H32), C26(H26), C33(H33)
6.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C14A(H14A,H14B,H14C), C12A(H12E,H12F,H12G), C10A(H10A,
 H10B,H10C), C9A(H9AA,H9AB,H9AC), C8A(H8AA,H8AB,H8AC), C7A(H7AA,H7AB,H7AC),
 C01(H01A,H01B,H01C), C08(H08A,H08B,H08C), C02(H02A,H02B,H02C), C04(H04A,H04B,
 H04C), C09(H09A,H09B,H09C), C09A(H09D,H09E,H09F), C04A(H04D,H04E,H04F)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'