Three novel polyoxoanion-supported compounds: confinement of polyoxoanions in Ni-containing rigid concave surfaces with enhanced NLO properties.
Dong, Yayu; Xu, Xiao; Zhou, Guangpeng; Miao, Hao; Hu, GongHao; Xu, Yan; Dalton transactions (Cambridge, England : 2003) 44 (2015) 18347–18353; doi:10.1039/c5dt02710a

data_7036397
_publ_section_title
;
 Three novel polyoxoanion-supported compounds: confinement of
 polyoxoanions in Ni-containing rigid concave surfaces with enhanced NLO
 properties.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18347
_journal_page_last               18353
_journal_paper_doi               10.1039/c5dt02710a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C48 H55 Mo12 N14 Ni2 O46.5 P'
_chemical_formula_weight         2871.73
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-09-01 deposited with the CCDC.
2015-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
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_cell_angle_gamma                90
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_cell_length_c                   24.310(4)
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_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.96
_cell_measurement_theta_min      2.20
_cell_volume                     8019(2)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_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  0.0468
_diffrn_reflns_av_unetI/netI     0.0675
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            58856
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.498
_diffrn_reflns_theta_min         1.199
_exptl_absorpt_coefficient_mu    2.390
_exptl_absorpt_correction_T_max  0.7624
_exptl_absorpt_correction_T_min  0.6867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.378
_exptl_crystal_description       strip
_exptl_crystal_F_000             5552
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_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.196
_refine_diff_density_min         -1.108
_refine_diff_density_rms         0.138
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.506(15)
_refine_ls_extinction_coef       0.000084(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2235
_refine_ls_number_reflns         26620
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0470P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0946
_refine_ls_wR_factor_ref         0.1018
_reflns_Friedel_coverage         0.951
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                21904
_reflns_number_total             26620
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02710a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7036396--7036398.cif.'
_cod_original_cell_volume        8020(2)
_cod_original_formula_sum        'C48 H55 Mo12 N14 Ni2 O46.50 P'
_cod_database_code               7036397
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.687
_shelx_estimated_absorpt_t_max   0.762
_shelx_res_checksum              52544