Synthesis of Bimetallic Bis(phenolate) N-Heterocyclic Carbene Lanthanide Complexes and Their Applications in the Ring-Opening Polymerization ofl-Lactide
Zhang, Min; Ni, Xufeng; Shen, Zhiquan; Organometallics 33 (2014) 6861–; doi:10.1021/om500930m

data_4084878
_publ_section_title
;
 Synthesis of Bimetallic Bis(phenolate) N-Heterocyclic Carbene Lanthanide
 Complexes and Their Applications in the Ring-Opening Polymerization
 ofl-Lactide
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6861
_journal_paper_doi               10.1021/om500930m
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety
'2(C68.33 H100.67 K La N4 O4.58), 0.83(C4 H8 O)'
_chemical_formula_sum            'C140 H208 K2 La2 N8 O10'
_chemical_formula_weight         2519.16
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-04-29
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                64.125(4)
_cell_angle_beta                 71.527(4)
_cell_angle_gamma                80.970(4)
_cell_formula_units_Z            1
_cell_length_a                   15.1703(7)
_cell_length_b                   15.8589(7)
_cell_length_c                   17.7284(7)
_cell_measurement_reflns_used    7750
_cell_measurement_temperature    170.1
_cell_measurement_theta_max      29.5235
_cell_measurement_theta_min      2.9406
_cell_volume                     3639.0(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      170.1
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0045713000
_diffrn_orient_matrix_UB_12      -0.0489654000
_diffrn_orient_matrix_UB_13      0.0242131000
_diffrn_orient_matrix_UB_21      -0.0325494000
_diffrn_orient_matrix_UB_22      0.0036211000
_diffrn_orient_matrix_UB_23      0.0373737000
_diffrn_orient_matrix_UB_31      -0.0367542000
_diffrn_orient_matrix_UB_32      -0.0078380000
_diffrn_orient_matrix_UB_33      -0.0127208000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_unetI/netI     0.0778
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24247
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.95
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.690
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.236
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     816
_refine_ls_number_reflns         13284
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0648P)^2^+1.2503P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1357
_reflns_number_gt                10732
_reflns_number_total             13284
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500930m_si_002.cif
_cod_data_source_block           140423_zm_0423_la
_cod_depositor_comments
'Adding full bibliography for 4084876--4084881.cif.'
_cod_database_code               4084878
_chemical_oxdiff_formula         'c10 h10 n2 o8 La1'
_reflns_odcompleteness_completeness 99.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Uiso/Uaniso restraints and constraints
C69 \\sim C68 \\sim C67 \\sim C70 \\sim C74 \\sim C72 \\sim C71 \\sim C73:
within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C62) = Uanis(C62A)
Uanis(C60) = Uanis(C60A)
Uanis(C61) = Uanis(C61A)
Uanis(K1A) = Uanis(K1)
3. Others
 Sof(K1)=Sof(O1)=Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(C68)=Sof(H68A)=Sof(H68B)=
 Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(C70)=Sof(H70A)=Sof(H70B)=1-FVAR(1)
 Sof(K1A)=Sof(O2)=Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(C72)=Sof(H72A)=Sof(H72B)=
 Sof(C73)=Sof(H73A)=Sof(H73B)=Sof(C74)=Sof(H74A)=Sof(H74B)=FVAR(1)
 Sof(C62A)=Sof(H62D)=Sof(H62E)=Sof(H62F)=Sof(C60A)=Sof(H60D)=Sof(H60E)=
 Sof(H60F)=Sof(C61A)=Sof(H61D)=Sof(H61E)=Sof(H61F)=1-FVAR(2)
 Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(H60C)=Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(H61C)=
 Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(H62C)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C11(H11A,H11B), C40(H40A,H40B),
 C41(H41A,H41B), C42(H42A,H42B), C44(H44A,H44B), C67(H67A,H67B), C68(H68A,H68B),
  C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B), C72(H72A,H72B), C73(H73A,
 H73B), C74(H74A,H74B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C13(H13), C15(H15), C36(H36), C38(H38), C46(H46), C48(H48)
4.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C),
 C32(H32A,H32B,H32C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,
 H54C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C60(H60A,
 H60B,H60C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C64(H64A,H64B,H64C),
 C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C62A(H62D,H62E,H62F), C60A(H60D,H60E,
 H60F), C61A(H61D,H61E,H61F)
;