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_7047454
_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         'C35.35 H40.3 Gd N0.35 O11 S0.65'
_chemical_formula_sum            'C35.35 H40.3 Gd N0.35 O11 S0.65'
_chemical_formula_weight         824.17
_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
_audit_creation_date             2018-06-16
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-06-21 deposited with the CCDC.
2018-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                110.47(3)
_cell_angle_beta                 103.78(2)
_cell_angle_gamma                95.51(3)
_cell_formula_units_Z            2
_cell_length_a                   8.544(7)
_cell_length_b                   14.813(14)
_cell_length_c                   16.466(16)
_cell_measurement_reflns_used    7518
_cell_measurement_temperature    250.1
_cell_measurement_theta_max      65.278
_cell_measurement_theta_min      3.020
_cell_volume                     1859(3)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      250.1
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0853
_diffrn_reflns_av_unetI/netI     0.0855
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20718
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        63.690
_diffrn_reflns_theta_max         63.690
_diffrn_reflns_theta_min         2.995
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    12.354
_exptl_absorpt_correction_T_max  0.6603
_exptl_absorpt_correction_T_min  0.3971
_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 0.0765 after correction.
The Ratio of minimum to maximum transmission is 0.6014.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_description       block
_exptl_crystal_F_000             834
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.093
_refine_diff_density_min         -0.792
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         6008
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0491
_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^)+(0.0807P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1272
_refine_ls_wR_factor_ref         0.1379
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4920
_reflns_number_total             6008
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03020k2.cif
_cod_data_source_block           EM44
_cod_depositor_comments
'Adding full bibliography for 7047449--7047454.cif.'
_cod_original_formula_sum        'C35.35 H40.30 Gd N0.35 O11 S0.65'
_cod_database_code               7047454
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.371
_shelx_estimated_absorpt_t_min   0.259
_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(C37) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: S1(0.65) N1(0.35) C36(0.35) H36(0.35) H35A(0.65) H35B(0.65)
 H35C(0.65) C37(0.35) H37A(0.35) H37B(0.35) H37C(0.35) C34(0.65) H34A(0.65)
 H34B(0.65) H34C(0.65)
4.a Rotating group:
 O1W(H1WA,H1WB)
4.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C21(H21A,H21B), C32(H32A,H32B)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C13(H13), C14(H14), C16(H16),
 C17(H17), C18(H18), C19(H19), C24(H24), C25(H25), C27(H27), C28(H28), C29(H29),
  C30(H30), C36(H36)
4.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C22(H22A,H22B,H22C), C33(H33A,H33B,H33C), C35(H35A,H35B,
 H35C), C37(H37A,H37B,H37C), C34(H34A,H34B,H34C)
;
_olex2_submission_original_sample_id EM44
_olex2_submission_special_instructions 'No special instructions were received'