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_7703981
_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         'C53 H82 La N3 O4, 2.5(C4 H8 O)'
_chemical_formula_sum            'C63 H102 La N3 O6.5'
_chemical_formula_weight         1144.38
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc24d36w
_audit_creation_date             2019-12-09
_audit_creation_method
;
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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   28.6963(3)
_cell_length_b                   28.6963(3)
_cell_length_c                   33.2864(6)
_cell_measurement_reflns_used    18481
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      29.4540
_cell_measurement_theta_min      3.4320
_cell_volume                     27410.6(6)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0374
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            62531
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         3.150
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92483
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             9760
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.989
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     662
_refine_ls_number_reflns         14002
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0464
_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^)+(0.0578P)^2^+106.6705P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1392
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10631
_reflns_number_total             14002
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00179a2.cif
_cod_data_source_block           g130426a
_cod_depositor_comments
'Adding full bibliography for 7703981--7703985.cif.'
_cod_original_cell_volume        27410.6(8)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_original_formula_sum        'C63 H102 La N3 O6.50'
_cod_database_code               7703981
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O8-C66 = O8-C69
 1.42 with sigma of 0.02
 C66-C67 = C67-C68 = C68-C69
 1.5 with sigma of 0.02
 C66-C68 = C67-C69
 2.49 with sigma of 0.02
 O8-C67 = O8-C68
 2.41 with sigma of 0.02
 C62-C64 = C65-C63
 2.49 with sigma of 0.02
 C62-C63 = C63-C64 = C64-C65
 1.5 with sigma of 0.02
 O7-C62 = O7-C65
 1.42 with sigma of 0.02
 C58-C60 = C61-C59
 2.49 with sigma of 0.02
 C58-C59 = C59-C60 = C60-C61
 1.5 with sigma of 0.02
 O6-C58 = O6-C61
 1.42 with sigma of 0.01
 O6-C60 = O6-C59
 2.41 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uiso(O8) = Uiso(C66) = Uiso(C67) = Uiso(C68) = Uiso(C69)
Uiso(C62) = Uiso(C63) = Uiso(C64) = Uiso(C65) = Uiso(O7)
Uiso(C58) = Uiso(C59) = Uiso(C60) = Uiso(C61) = Uiso(O6)
4. Others
 Fixed Sof: O6(0.5) C58(0.5) H58A(0.5) H58B(0.5) C59(0.5) H59A(0.5) H59B(0.5)
 C60(0.5) H60A(0.5) H60B(0.5) C61(0.5) H61A(0.5) H61B(0.5) O7(0.5) C62(0.5)
 H62A(0.5) H62B(0.5) C63(0.5) H63A(0.5) H63B(0.5) C64(0.5) H64A(0.5) H64B(0.5)
 C65(0.5) H65A(0.5) H65B(0.5) O8(0.5) C68(0.5) H68A(0.5) H68B(0.5) C66(0.5)
 H66A(0.5) H66B(0.5) C67(0.5) H67A(0.5) H67B(0.5) C69(0.5) H69A(0.5) H69B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C54(H54A,H54B), C55(H55A,
 H55B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B),
 C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B),
  C65(H65A,H65B), C68(H68A,H68B), C66(H66A,H66B), C67(H67A,H67B), C69(H69A,
 H69B), C53(H53A,H53B), C50(H50A,H50B), C52(H52A,H52B), C51(H51A,H51B),
 C11(H11A,H11B)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C22(H22), C24(H24), C26(H26), C37(H37), C39(H39)
5.c 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), C42(H42A,H42B,H42C), C43(H43A,
 H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C32(H32A,H32B,H32C), C19(H19A,H19B,
 H19C), C34(H34A,H34B,H34C), C18(H18A,H18B,H18C), C33(H33A,H33B,H33C), C17(H17A,
 H17B,H17C)
;
_olex2_submission_special_instructions 'No special instructions were received'