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_7040448
_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 H106 Er2 N6 O4 Si4'
_chemical_formula_sum            'C60 H106 Er2 N6 O4 Si4'
_chemical_formula_weight         1422.38
_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             2015-10-29
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-04-25 deposited with the CCDC.
2016-08-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.6740(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.625(3)
_cell_length_b                   15.0990(16)
_cell_length_c                   33.700(4)
_cell_measurement_reflns_used    9732
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      27.60
_cell_measurement_theta_min      2.26
_cell_volume                     14045(3)
_computing_cell_refinement       'SAINT v7.34A (Bruker, 200?)'
_computing_data_reduction        'SAINT v7.34A (Bruker, 200?)'
_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    'ShelXT (Sheldrick, 2015)'
_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_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            109633
_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         26.372
_diffrn_reflns_theta_min         1.476
_exptl_absorpt_coefficient_mu    2.486
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       block
_exptl_crystal_F_000             5856
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.198
_refine_diff_density_min         -2.028
_refine_diff_density_rms         0.107
_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     1442
_refine_ls_number_reflns         28646
_refine_ls_number_restraints     467
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0373P)^2^+30.2922P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0896
_refine_ls_wR_factor_ref         0.0989
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22015
_reflns_number_total             28646
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02922a2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7040444--7040455.cif.'
_cod_database_code               7040448
_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. 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
3. Others
 Sof(H02Y)=Sof(HG)=Sof(HJ)=Sof(HK)=Sof(C3A)=Sof(H3AB)=Sof(H3AC)=Sof(C0)=
 Sof(H0A)=Sof(H0B)=1-FVAR(1)
 Sof(H02W)=Sof(H02X)=Sof(H02)=Sof(HI)=Sof(C047)=Sof(H04E)=Sof(H04F)=Sof(C3)=
 Sof(H3A)=Sof(H3B)=FVAR(1)
 Sof(H02L)=Sof(H02M)=Sof(H3GA)=Sof(H4GA)=Sof(C0AA)=Sof(H0AB)=Sof(H0AC)=1-FVAR(2)
 Sof(H02J)=Sof(H02K)=Sof(H03X)=Sof(H03Y)=Sof(C03X)=Sof(H8AA)=Sof(H0JA)=FVAR(2)
 Sof(HT)=Sof(HU)=Sof(H1IA)=Sof(H2IA)=Sof(C1)=Sof(H1A)=Sof(H1B)=1-FVAR(3)
 Sof(H0CA)=Sof(HS)=Sof(H0EA)=Sof(H0IA)=Sof(C041)=Sof(H04I)=Sof(H04J)=FVAR(3)
 Sof(H0GA)=Sof(H1GA)=Sof(H1JA)=Sof(H2JA)=Sof(C2)=Sof(H2A)=Sof(H2B)=1-FVAR(4)
 Sof(H2DA)=Sof(H9FA)=Sof(H4EA)=Sof(H3JA)=Sof(C045)=Sof(H04P)=Sof(H04Q)=FVAR(4)
4.a Ternary CH refined with riding coordinates:
 C017(H017), C018(H018), C01I(H01P), C01J(H01J), C01U(H01), C01X(H01X),
 C02A(H2BA), C02O(H7BA)
4.b Secondary CH2 refined with riding coordinates:
 C01F(H01B,H01D), C01L(H01T,H01U), C01S(H01Y,H), C01V(H01E,H01F), C01W(H01H,
 H01I), C021(H9AA,HA), C022(H02A,H02B), C023(H02C,H02D), C024(H02E,H02F),
 C026(H0BA,HB), C028(H02J,H02K), C028(H02L,H02M), C02B(H02N,H02O), C02C(H02P,
 H02Q), C02E(H02U,H02V), C02F(H3BA,HE), C02G(H4BA,HF), C02H(H02Y,HG), C02H(H02W,
 H02X), C02J(H02Z,HH), C02K(H02,HI), C02K(HJ,HK), C02L(H0AA,HL), C02P(H8BA,HQ),
 C02Q(H2AA,HR), C02S(H0CA,HS), C02S(HT,HU), C02T(H3AA,HV), C02U(H1CA,HW),
 C02V(H2CA,HX), C02W(H3CA,HY), C030(H03A,H03B), C032(H6CA,H1FA), C033(H03F,
 H03G), C034(H03H,H03I), C035(H7CA,H2FA), C036(H03J,H03K), C037(H8CA,H3FA),
 C03E(H1DA,H8FA), C03F(H2DA,H9FA), C03F(H0GA,H1GA), C03G(H3DA,H2GA), C03H(H03X,
 H03Y), C03H(H3GA,H4GA), C03I(H4DA,H5GA), C03J(H5DA,H6GA), C03N(H8DA,H3HA),
 C03O(H03,H4HA), C03R(H9DA,H9HA), C03S(H0EA,H0IA), C03S(H1IA,H2IA), C03W(H7AA,
 H9IA), C03X(H8AA,H0JA), C03Y(H1JA,H2JA), C03Y(H4EA,H3JA), C03Z(H5EA,H4JA),
 C040(H04G,H04H), C041(H04I,H04J), C042(H04K,H04L), C043(H04A,H04B), C045(H04P,
 H04Q), C046(H04C,H04D), C047(H04E,H04F), C3(H3A,H3B), C3A(H3AB,H3AC), C0(H0A,
 H0B), C0AA(H0AB,H0AC), C1(H1A,H1B), C2(H2A,H2B)
4.c Aromatic/amide H refined with riding coordinates:
 C013(H013), C014(H014), C016(H016), C01A(H01A), C01B(H01K), C01C(H01C),
 C01E(H01L), C01G(H01G), C01H(H01M), C01K(H01S), C01M(H01V), C01N(H01N),
 C01O(H01O), C01P(H01W), C01Q(H01Q), C01R(H01R), C01T(H01Z), C020(H020),
 C02I(H5BA), C02R(H9BA)
4.d Idealised Me refined as rotating group:
 C027(H02G,H02H,H02I), C029(H1BA,HC,HD), C02D(H02R,H02S,H02T), C02M(H6BA,HM,
 HN), C02N(H1AA,HO,HP), C02X(H4AA,HZ,H6EA), C02Y(H4CA,H7EA,H8EA), C02Z(H5CA,
 H9EA,H0FA), C031(H03C,H03D,H03E), C038(H03L,H03M,H03N), C039(H03O,H03P,H03Q),
 C03A(H03R,H03S,H03T), C03B(H03U,H03V,H03W), C03C(H9CA,H4FA,H5FA), C03D(H0DA,
 H6FA,H7FA), C03K(H6DA,H7GA,H8GA), C03L(H03Z,H9GA,H0HA), C03M(H7DA,H1HA,H2HA),
 C03P(H5AA,H5HA,H6HA), C03Q(H6AA,H7HA,H8HA), C03T(H1EA,H3IA,H4IA), C03U(H2EA,
 H5IA,H6IA), C03V(H3EA,H7IA,H8IA), C044(H04M,H04N,H04O)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'