Layered V-B-O polyoxometalate nets linked by diethylenetriamine complexes with dangling amine groups.
Chen, Hong; Zhang, Yunfeng; Yu, Zheng-Bao; Sun, Junliang; Dalton transactions (Cambridge, England : 2003) 43 (2014) 15283–15286; doi:10.1039/c4dt01533a

data_7032081
_publ_section_title
;
 Layered V-B-O polyoxometalate nets linked by diethylenetriamine complexes
 with dangling amine groups.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15283
_journal_page_last               15286
_journal_paper_doi               10.1039/c4dt01533a
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C24 H86 B6 Cu3 N18 O73 P12 V12'
_chemical_formula_weight         3033.51
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   18.0955(2)
_cell_length_b                   18.0955(2)
_cell_length_c                   30.0074(5)
_cell_measurement_temperature    298(2)
_cell_volume                     8509.42(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0610
_diffrn_reflns_av_sigmaI/netI    0.0364
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            39485
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         4.28
_exptl_absorpt_coefficient_mu    1.761
_exptl_absorpt_correction_T_max  0.9171
_exptl_absorpt_correction_T_min  0.8165
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.776
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4539
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.048
_refine_diff_density_min         -1.264
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         3863
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0674
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1219P)^2^+47.3114P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2060
_refine_ls_wR_factor_ref         0.2177
_reflns_number_gt                3035
_reflns_number_total             3863
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt01533a2.cif
_cod_data_source_block           r-3sqd
_cod_depositor_comments
'Adding full bibliography for 7032080--7032082.cif.'
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7032081