Lanthanide derivatives comprising arylhydrazones of β-diketones: cooperative E/Z isomerization and catalytic activity in nitroaldol reaction.
Mahmudov, Kamran T.; Guedes da Silva, M Fátima C; Sutradhar, Manas; Kopylovich, Maximilian N.; Huseynov, Fatali E.; Shamilov, Nazim T.; Voronina, Anna A.; Buslaeva, Tatyana M.; Pombeiro, Armando J. L.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 5602–5610; doi:10.1039/c4dt03788j

data_7033830
_publ_section_title
;
 Lanthanide derivatives comprising arylhydrazones of \b-diketones:
 cooperative E/Z isomerization and catalytic activity in nitroaldol
 reaction.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5602
_journal_page_last               5610
_journal_paper_doi               10.1039/c4dt03788j
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         '3(C16 H12 Cl N2 O6 S), H18 O9 Sm, 2(H2 O)'
_chemical_formula_sum            'C48 H58 Cl3 N6 O29 S3 Sm'
_chemical_formula_weight         1535.88
_chemical_name_systematic
;
 ?
;
_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_method           SHELXL-2013
_audit_update_record
;
2015-01-19 deposited with the CCDC.
2015-01-26 downloaded from the CCDC.
;
_cell_angle_alpha                76.866(2)
_cell_angle_beta                 77.383(2)
_cell_angle_gamma                87.504(2)
_cell_formula_units_Z            2
_cell_length_a                   11.2987(5)
_cell_length_b                   12.1861(5)
_cell_length_c                   23.7103(10)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      22.31
_cell_measurement_theta_min      2.41
_cell_volume                     3102.4(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1997)'
_diffrn_ambient_temperature      299(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II PHOTON 100 detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0912
_diffrn_reflns_av_unetI/netI     0.0721
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            63896
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_min         2.616
_exptl_absorpt_coefficient_mu    1.269
_exptl_absorpt_correction_T_max  0.892
_exptl_absorpt_correction_T_min  0.772
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             1562
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.090
_platon_squeeze_details
;
 Although data resulting from the use of Platon Squeeze
 are indicated the corrected hkl file did not improve the final
 R factor and electrons could not be removed from the model.
 Electron density close to O6 could not be acertained.
;
_refine_diff_density_max         3.699
_refine_diff_density_min         -0.742
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     870
_refine_ls_number_reflns         11370
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1198
_refine_ls_R_factor_gt           0.0827
_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^)+(0.1435P)^2^+7.0688P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2135
_refine_ls_wR_factor_ref         0.2354
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7779
_reflns_number_total             11370
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03788j2.cif
_cod_data_source_block           Compound2
_cod_depositor_comments
'Adding full bibliography for 7033829--7033830.cif.'
_cod_database_code               7033830
_shelx_estimated_absorpt_t_min   0.768
_shelx_estimated_absorpt_t_max   0.894
_shelxl_version_number           2013-4
_shelx_res_checksum              80621