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_7703984
_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         'C72 H112 La2 N6 O6, 4(C4 H8 O)'
_chemical_formula_sum            'C88 H144 La2 N6 O10'
_chemical_formula_weight         1723.90
_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   geom
_audit_block_doi                 10.5517/ccdc.csd.cc24d39z
_audit_creation_date             2019-12-09
_audit_creation_method
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-15 deposited with the CCDC.	2020-04-06 downloaded from the CCDC.
;
_cell_angle_alpha                95.089(3)
_cell_angle_beta                 107.153(4)
_cell_angle_gamma                104.378(4)
_cell_formula_units_Z            1
_cell_length_a                   12.0092(6)
_cell_length_b                   13.9383(6)
_cell_length_c                   14.9998(5)
_cell_measurement_reflns_used    8742
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      25.6950
_cell_measurement_theta_min      3.3590
_cell_volume                     2288.12(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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      223.15
_diffrn_detector_area_resol_mean 10.4692
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1473
_diffrn_reflns_av_unetI/netI     0.1454
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20951
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_min         2.873
_exptl_absorpt_coefficient_mu    0.977
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark yellow'
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.886
_refine_diff_density_min         -1.996
_refine_diff_density_rms         0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         8676
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.1096
_refine_ls_R_factor_gt           0.0944
_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^)+(0.1400P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2344
_refine_ls_wR_factor_ref         0.2600
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6643
_reflns_number_total             8676
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00179a2.cif
_cod_data_source_block           g130927a
_cod_depositor_comments
'Adding full bibliography for 7703981--7703985.cif.'
_cod_original_cell_volume        2288.12(18)
_cod_database_code               7703984
_shelx_shelxl_version_number     2016/4
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C16-C17 = C16-C18 = C16-C19 = C16-C17A = C16-C18A = C16-C19A
 1.53 with sigma of 0.02
 C31-C32 = C31-C32A = C31-C33 = C31-C33A = C31-C34 = C31-C34A
 1.53 with sigma of 0.02
 C41-C42 = C42-C43 = C43-C44
 1.52 with sigma of 0.02
 O5-C41 = O5-C44
 1.42 with sigma of 0.02
 C37-C38 = C38-C39 = C39-C40
 1.52 with sigma of 0.02
 O4-C37 = O4-C40
 1.42 with sigma of 0.02
 C35-C36 \\sim C35-C36A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C36) = Uanis(C36A)
Uanis(C17) = Uanis(C18) = Uanis(C19) = Uanis(C17A) = Uanis(C18A) = Uanis(C19A)
Uanis(C32) = Uanis(C33) = Uanis(C34) = Uanis(C32A) = Uanis(C33A) = Uanis(C34A)
Uiso(C41) = Uiso(C42) = Uiso(C43) = Uiso(C44)
Uiso(C37) = Uiso(C38) = Uiso(C39) = Uiso(C40)
4. 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) C32(0.5) H32A(0.5) H32B(0.5) H32C(0.5) C33(0.5)
 H33A(0.5) H33B(0.5) H33C(0.5) C34(0.5) H34A(0.5) H34B(0.5) H34C(0.5) C32A(0.5)
 H32D(0.5) H32E(0.5) H32F(0.5) C33A(0.5) H33D(0.5) H33E(0.5) H33F(0.5)
 C34A(0.5) H34D(0.5) H34E(0.5) H34F(0.5) H35A(0.5) H35B(0.5) H35C(0.5)
 H35D(0.5) C36(0.5) H36A(0.5) H36B(0.5) H36C(0.5) C36A(0.5) H36D(0.5) H36E(0.5)
 H36F(0.5)
5.a Ternary CH refined with riding coordinates:
 N2(H2)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C35(H35A,H35B), C35(H35C,
 H35D), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B),
 C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B)
5.c 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), C32(H32A,H32B,H32C),
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C32A(H32D,H32E,H32F), C33A(H33D,H33E,
 H33F), C34A(H34D,H34E,H34F), C36(H36A,H36B,H36C), C36A(H36D,H36E,H36F)
5.d Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C11(H11), C22(H22), C24(H24), C26(H26)
5.e 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)
;
_olex2_submission_special_instructions 'No special instructions were received'