Synthesis, structure and magnetic investigations of dinuclear lanthanide complexes based on 2-ethoxycinnamate.
Zouzou, Amina; Beghidja, Adel; Long, Jérôme; Beghidja, Chahrazed; Gándara, Felipe; Guari, Yannick; Larionova, Joulia; Dalton transactions (Cambridge, England : 2003) 47 (2018) 13647–13656; doi:10.1039/c8dt03020k

data_7047453
_publ_section_title
;
 Synthesis, structure and magnetic investigations of dinuclear lanthanide
 complexes based on 2-ethoxycinnamate.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13647
_journal_page_last               13656
_journal_paper_doi               10.1039/c8dt03020k
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C36 H42 N O11 Tb'
_chemical_formula_sum            'C36 H42 N O11 Tb'
_chemical_formula_weight         823.62
_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   mixed
_atom_sites_solution_primary     direct
_audit_update_record
;
2018-06-21 deposited with the CCDC.
2018-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                60.453(2)
_cell_angle_beta                 74.399(2)
_cell_angle_gamma                89.018(2)
_cell_formula_units_Z            2
_cell_length_a                   9.0353(3)
_cell_length_b                   15.2780(6)
_cell_length_c                   15.3738(6)
_cell_measurement_reflns_used    9859
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      64.710
_cell_measurement_theta_min      3.357
_cell_volume                     1761.24(12)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'SIR2004 (Burla et al.,  2007)'
_diffrn_ambient_temperature      173.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0639
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            33016
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        64.704
_diffrn_reflns_theta_max         64.704
_diffrn_reflns_theta_min         3.357
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.388
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7187
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1172 before and 0.0809 after correction.
The Ratio of minimum to maximum transmission is 0.7187.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_description       prism
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.850
_refine_diff_density_min         -0.751
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         5799
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0713P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1006
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5399
_reflns_number_total             5799
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03020k2.cif
_cod_data_source_block           em7
_cod_depositor_comments
'Adding full bibliography for 7047449--7047454.cif.'
_cod_database_code               7047453
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.369
_shelx_estimated_absorpt_t_min   0.287
_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, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C33B) = Uanis(C33A)
Uanis(C32A) = Uanis(C32B)
3. Rigid body (RIGU) restrains
 C26, C27, C28, C29, C30, C31
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C32A)=Sof(H32A)=Sof(H32B)=Sof(C33A)=Sof(H33A)=Sof(H33B)=Sof(H33C)=1-FVAR(1)
 Sof(C32B)=Sof(H32C)=Sof(H32D)=Sof(C33B)=Sof(H33D)=Sof(H33E)=Sof(H33F)=FVAR(1)
5.a Rotating group:
 O1W(H1WA,H1WB)
5.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C32A(H32A,H32B), C32B(H32C,H32D)
5.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C14(H14), C17(H17), C27(H27), C28(H28), C29(H29),
 C30(H30)
5.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C22(H22A,H22B,H22C), C33A(H33A,H33B,H33C), C33B(H33D,
 H33E,H33F), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C)
;
_olex2_submission_original_sample_id EM7
_olex2_submission_special_instructions 'No special instructions were received'