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_2021295
_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
'[Dy (C11 H15 N7 O2) (H2 O)3] [P Mo12 O40], 5H2 O'
_chemical_formula_sum            'C11 H31 Dy Mo12 N7 O50 P'
_chemical_formula_weight         2406.18
_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>']dysprosium(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                80.092(3)
_cell_angle_beta                 87.602(3)
_cell_angle_gamma                75.013(2)
_cell_formula_units_Z            2
_cell_length_a                   11.566(3)
_cell_length_b                   15.218(3)
_cell_length_c                   15.257(3)
_cell_measurement_reflns_used    7279
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.777
_cell_measurement_theta_min      2.274
_cell_volume                     2555.4(10)
_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
;
SHELXTL (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker Apex2 CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18194
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         1.405
_exptl_absorpt_coefficient_mu    4.439
_exptl_absorpt_correction_T_max  0.665
_exptl_absorpt_correction_T_min  0.641
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2005)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.127
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             2262
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.100
_refine_diff_density_max         2.325
_refine_diff_density_min         -1.512
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     741
_refine_ls_number_reflns         9300
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0636P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1026
_refine_ls_wR_factor_ref         0.1109
_reflns_number_gt                7280
_reflns_number_total             9300
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jr3003sup1.cif
_cod_data_source_block           a-2
_cod_original_cell_volume        2555.3(10)
_cod_database_code               2021295
_cod_database_fobs_code          2021295
_shelx_estimated_absorpt_t_min   0.641
_shelx_estimated_absorpt_t_max   0.665
_shelx_hkl_checksum              27250
_shelx_res_checksum              56734