Design, synthesis and excellent third-order NLO properties of two new polyoxometalates constructed from Keggin polyanions bonded by a solvent molecule.
Miao, Hao; Dong, Yayu; Chen, Ziwang; He, Xingxiang; Hu, Gonghao; Xu, Yan; Dalton transactions (Cambridge, England : 2003) 45 (2016) 12717–12722; doi:10.1039/c6dt02320g

data_7039912
_publ_section_title
;
 Design, synthesis and excellent third-order NLO properties of two new
 polyoxometalates constructed from Keggin polyanions bonded by a solvent
 molecule.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12717
_journal_page_last               12722
_journal_paper_doi               10.1039/c6dt02320g
_journal_volume                  45
_journal_year                    2016
_chemical_absolute_configuration L
_chemical_formula_sum            'C28.5 H39 Co N5 O40.5 P W11'
_chemical_formula_weight         3211.89
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-07-05 deposited with the CCDC.
2016-07-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.509(2)
_cell_length_b                   17.921(3)
_cell_length_c                   26.488(5)
_cell_measurement_reflns_used    2978
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.32
_cell_volume                     6412.6(19)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0799
_diffrn_reflns_av_unetI/netI     0.0785
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            44169
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.024
_diffrn_reflns_theta_max         25.024
_diffrn_reflns_theta_min         1.372
_exptl_absorpt_coefficient_mu    20.010
_exptl_absorpt_correction_T_max  0.1973
_exptl_absorpt_correction_T_min  0.1538
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    3.327
_exptl_crystal_description       Block
_exptl_crystal_F_000             5700
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.120
_refine_diff_density_max         3.254
_refine_diff_density_min         -2.992
_refine_diff_density_rms         0.412
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.50(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     803
_refine_ls_number_reflns         11291
_refine_ls_number_restraints     473
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1407
_refine_ls_wR_factor_ref         0.1610
_reflns_Friedel_coverage         0.814
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                8589
_reflns_number_total             11291
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02320g2.cif
_cod_data_source_block           mh-37
_cod_depositor_comments
'Adding full bibliography for 7039911--7039912.cif.'
_cod_original_cell_volume        6412.7(19)
_cod_original_formula_sum        'C28.50 H39 Co N5 O40.50 P W11'
_cod_database_code               7039912
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.153
_shelx_estimated_absorpt_t_max   0.197
_shelx_res_checksum              69519