Lanthanum complexes stabilized by a pentadentate Schiff-base ligand: synthesis, characterization, and reactivity in statistical copolymerization of ε-caprolactone and l-lactide.
Shao, Jingjing; Zhou, Hairong; Wang, Yaorong; Luo, Yunjie; Yao, Yingming; Dalton transactions (Cambridge, England : 2003) 49 (2020) 5842–5850; doi:10.1039/d0dt00179a

data_7703982
_publ_section_title
;
 Lanthanum complexes stabilized by a pentadentate Schiff-base ligand:
 synthesis, characterization, and reactivity in statistical
 copolymerization of \e-caprolactone and l-lactide.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5842
_journal_page_last               5850
_journal_paper_doi               10.1039/d0dt00179a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C42 H68 La N3 O4'
_chemical_formula_sum            'C42 H68 La N3 O4'
_chemical_formula_weight         817.90
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc24d3b0
_audit_creation_date             2019-12-09
_audit_creation_method
;
Olex2 1.3-alpha
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-01-15 deposited with the CCDC.	2020-04-06 downloaded from the CCDC.
;
_cell_angle_alpha                101.370(3)
_cell_angle_beta                 105.032(4)
_cell_angle_gamma                92.632(3)
_cell_formula_units_Z            2
_cell_length_a                   10.3685(4)
_cell_length_b                   13.2339(5)
_cell_length_c                   18.9841(8)
_cell_measurement_reflns_used    7220
_cell_measurement_temperature    223.15
_cell_measurement_theta_max      28.4130
_cell_measurement_theta_min      3.7720
_cell_volume                     2453.41(18)
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      223.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0529
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22665
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.157
_exptl_absorpt_coefficient_mu    0.906
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76643
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.107
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.630
_refine_diff_density_min         -0.772
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         9959
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+1.9956P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1058
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8547
_reflns_number_total             9959
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00179a2.cif
_cod_data_source_block           g130524b_sq
_cod_depositor_comments
'Adding full bibliography for 7703981--7703985.cif.'
_cod_original_cell_volume        2453.43(18)
_cod_database_code               7703982
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H2-N2
 0.9 with sigma of 0.02
 C16-C17 \\sim C16-C18 \\sim C16-C19 \\sim C16-C17A \\sim C16-C18A \\sim
C16-C19A
 with sigma of 0.02
 C35-C36 \\sim C35-C37 \\sim C35-C38 \\sim C35-C36A \\sim C35-C37A \\sim
C35-C38A
 with sigma of 0.02
3. Rigid bond restraints
 C35, C36, C37, C38
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C17) = Uanis(C18) = Uanis(C19) = Uanis(C17A) = Uanis(C18A) = Uanis(C19A)
Uanis(C36) = Uanis(C37) = Uanis(C38) = Uanis(C36A) = Uanis(C37A) = Uanis(C38A)
5. Others
 Fixed Sof: C17(0.5) H17A(0.5) H17B(0.5) H17C(0.5) C18(0.5) H18A(0.5)
 H18B(0.5) H18C(0.5) C19(0.5) H19A(0.5) H19B(0.5) H19C(0.5) C17A(0.5) H17D(0.5)
 H17E(0.5) H17F(0.5) C18A(0.5) H18D(0.5) H18E(0.5) H18F(0.5) C19A(0.5)
 H19D(0.5) H19E(0.5) H19F(0.5) C36(0.5) H36A(0.5) H36B(0.5) H36C(0.5) C37(0.5)
 H37A(0.5) H37B(0.5) H37C(0.5) C38(0.5) H38A(0.5) H38B(0.5) H38C(0.5) C36A(0.5)
 H36D(0.5) H36E(0.5) H36F(0.5) C37A(0.5) H37D(0.5) H37E(0.5) H37F(0.5)
 C38A(0.5) H38D(0.5) H38E(0.5) H38F(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C39(H39A,H39B), C40(H40A,
 H40B), C41(H41A,H41B), C42(H42A,H42B)
6.b Me refined with riding coordinates:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C17A(H17D,H17E,
 H17F), C18A(H18D,H18E,H18F), C19A(H19D,H19E,H19F), C36(H36A,H36B,H36C),
 C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C36A(H36D,H36E,H36F), C37A(H37D,H37E,
 H37F), C38A(H38D,H38E,H38F)
6.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C11(H11), C22(H22), C24(H24), C26(H26)
6.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              760
_shelx_fab_checksum              10195
_olex2_submission_special_instructions 'No special instructions were received'