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_7703985
_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         'C41 H58 La N3 O3, 1.5(C4 H8 O)'
_chemical_formula_sum            'C47 H70 La N3 O4.5'
_chemical_formula_weight         887.97
_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.cc24d38y
_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                114.717(4)
_cell_angle_beta                 101.976(4)
_cell_angle_gamma                104.959(3)
_cell_formula_units_Z            2
_cell_length_a                   12.9998(5)
_cell_length_b                   14.5735(5)
_cell_length_c                   15.2374(7)
_cell_measurement_reflns_used    9081
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.6630
_cell_measurement_theta_min      3.2470
_cell_volume                     2364.1(2)
_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  0.0336
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23213
_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         26.372
_diffrn_reflns_theta_min         2.839
_exptl_absorpt_coefficient_mu    0.947
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97294
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         1.187
_refine_diff_density_min         -1.014
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         9648
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0542P)^2^+2.7195P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1140
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8267
_reflns_number_total             9648
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00179a2.cif
_cod_data_source_block           g130704a
_cod_depositor_comments
'Adding full bibliography for 7703981--7703985.cif.'
_cod_original_cell_volume        2364.13(18)
_cod_original_formula_sum        'C47 H70 La N3 O4.50'
_cod_database_code               7703985
_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 N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C46-C47 = C47-C48 = C48-C49
 1.52 with sigma of 0.02
 O5-C46 = O5-C49
 1.42 with sigma of 0.02
 H2-N2
 0.9 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uiso(O5) = Uiso(C46) = Uiso(C47) = Uiso(C48) = Uiso(C49)
4. Others
 Fixed Sof: O5(0.5) C46(0.5) H46A(0.5) H46B(0.5) C47(0.5) H47A(0.5) H47B(0.5)
 C48(0.5) H48A(0.5) H48B(0.5) C49(0.5) H49A(0.5) H49B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C35(H35A,H35B), C46(H46A,
 H46B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B), C8AA(H8AA,H8AB),
 C0BA(H0BA,H0BB), C7AA(H7AA,H7AB), C9AA(H9AA,H9AB)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C11(H11), C22(H22), C24(H24), C26(H26), C37(H37), C38(H38),
 C39(H39), C40(H40), C41(H41)
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), C0AA(H0AA,H0AB,H0AC),
 C2AA(H2AA,H2AB,H2AC), C1AA(H1AA,H1AB,H1AC), C4AA(H4AA,H4AB,H4AC), C5AA(H5AA,
 H5AB,H5AC), C3AA(H3AA,H3AB,H3AC)
;
_olex2_submission_special_instructions 'No special instructions were received'