Assembly of chainlike polyoxometalate-based lanthanide complexes in one-pot reaction system
Feng, Xiao-Jia; Han, Hua-Yan; Wang, Yong-Hui; Li, Lu-Lu; Li, Yang-Guang; Wang, En-Bo; CrystEngComm 15 (2013) 7267–; doi:10.1039/c3ce40686e

data_7210307
_publ_section_title
;
 Assembly of chainlike polyoxometalate-based lanthanide complexes in
 one-pot reaction system
;
_journal_issue                   36
_journal_name_full               CrystEngComm
_journal_page_first              7267
_journal_paper_doi               10.1039/c3ce40686e
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C10 H134 As4 N2 Na10 Nd6 O214 W44'
_chemical_formula_weight         13191.61
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.8410(10)
_cell_angle_beta                 83.3810(10)
_cell_angle_gamma                87.2270(10)
_cell_formula_units_Z            1
_cell_length_a                   15.4412(12)
_cell_length_b                   19.3382(15)
_cell_length_c                   22.4967(17)
_cell_measurement_reflns_used    33554
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.15
_cell_volume                     6521.1(9)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL-PLUS (Sheldrick, 1990)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0515
_diffrn_reflns_av_sigmaI/netI    0.1225
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33161
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    21.098
_exptl_absorpt_correction_T_max  0.0808
_exptl_absorpt_correction_T_min  0.0667
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            light-purple
_exptl_crystal_density_diffrn    3.359
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5778
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_platon_squeeze_details
;
;
_refine_diff_density_max         2.498
_refine_diff_density_min         -2.070
_refine_diff_density_rms         0.406
_refine_ls_extinction_coef       0.000009(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1237
_refine_ls_number_reflns         22640
_refine_ls_number_restraints     354
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0561
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1297
_refine_ls_wR_factor_ref         0.1406
_reflns_number_gt                13956
_reflns_number_total             22640
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce40686e.txt
_cod_data_source_block           f4a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        6521.2(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7210307