Two new POM-based compounds modified by lanthanide–Schiff base complexes with interesting NLO properties
Luo, Xi-Ming; Cui, Chen-Hui; Cao, Jia-Peng; Lin, Qing-Fang; Xu, Yan; Acta Crystallographica Section C 74 (2018) –; doi:10.1107/S2053229618011853

data_2021294
_publ_section_title
;
 Two new POM-based compounds modified by lanthanide--Schiff base complexes
 with interesting NLO properties
;
_journal_coeditor_code           JR3003
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229618011853
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac
'[Tb (C11 H15 N7 O2) (H2 O)3] [P Mo12 O40], 5H2 O'
_chemical_formula_sum            'C11 H31 Mo12 N7 O50 P Tb'
_chemical_formula_weight         2402.60
_chemical_name_systematic
;{Triaqua[2,6-diacetylpyridine
bis(semicarbazone)-\k^5^<i>O</i>,<i>N</i>,<i>N</i>',<i>N</i>'',<i>O</i>']terbium(III)}-\m-oxido-[tricosa-\m~2~-oxido-dodecaoxido-\m~12~-phosphato-dodecamolybdenum(VI)] pentahydrate
;
_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-2014/7
_cell_angle_alpha                80.195(3)
_cell_angle_beta                 87.940(4)
_cell_angle_gamma                75.052(4)
_cell_formula_units_Z            2
_cell_length_a                   11.594(4)
_cell_length_b                   15.198(5)
_cell_length_c                   15.292(5)
_cell_measurement_reflns_used    9457
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.055
_cell_measurement_theta_min      2.282
_cell_volume                     2565.2(15)
_computing_cell_refinement
;
SAINT (Bruker, 2005)
;
_computing_data_collection
;
APEX2 (Bruker, 2005)
;
_computing_data_reduction
;
SAINT (Bruker, 2005)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18755
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         1.351
_exptl_absorpt_coefficient_mu    4.344
_exptl_absorpt_correction_T_max  0.624
_exptl_absorpt_correction_T_min  0.562
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2005)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.111
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             2260
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.734
_refine_diff_density_min         -1.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     749
_refine_ls_number_reflns         9401
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0302
_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^)+(0.0337P)^2^+1.8510P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0816
_reflns_number_gt                8029
_reflns_number_total             9401
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jr3003sup1.cif
_cod_data_source_block           a-1
_cod_original_cell_volume        2565.0(13)
_cod_database_code               2021294
_cod_database_fobs_code          2021294
_shelx_estimated_absorpt_t_min   0.562
_shelx_estimated_absorpt_t_max   0.624
_shelx_hkl_checksum              31918
_shelx_res_checksum              33965