Novel charge transfer supramolecular assemblies with Keggin anions and 2-amino-5-nitropyridine.
Gamelas, J. A. F.; Santos, F. M.; Felix, V.; Cavaleiro, A. M. V.; de Matos Gomes, E.; Belsley, M.; Drew, M. G. B.; Dalton transactions (Cambridge, England : 2003)  (2006) 1197–1203; doi:10.1039/b508986g

data_7006374
_publ_section_title
;
 Novel charge transfer supramolecular assemblies with Keggin anions and
 2-amino-5-nitropyridine.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1197
_journal_page_last               1203
_journal_paper_doi               10.1039/b508986g
_journal_year                    2006
_chemical_formula_sum            'C21 H32 Mo12 N12 O51 P'
_chemical_formula_weight         2450.84
_chemical_name_systematic
;
?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.699(14)
_cell_length_b                   20.905(23)
_cell_length_c                   22.741(25)
_cell_measurement_reflns_used    35464
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.85
_cell_measurement_theta_min      1.32
_cell_volume                     6513(12)
_computing_cell_refinement       XDS
_computing_data_collection       'XDS (Kabsch, 1991)'
_computing_data_reduction        XDS
_computing_molecular_graphics    PLATON(Spek,1994)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Marresearch Image Plate'
_diffrn_measurement_method
'95 frames at 2o intervals, counting time 2 min.'
_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  0.0452
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            35464
_diffrn_reflns_theta_full        25.85
_diffrn_reflns_theta_max         25.85
_diffrn_reflns_theta_min         1.32
_exptl_absorpt_coefficient_mu    2.369
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.731
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Walker et al., Acta Cryst 1983 A39 158'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.500
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4676
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.348
_refine_diff_density_min         -1.369
_refine_diff_density_rms         0.459
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.49(6)
_refine_ls_extinction_coef       0.00167(15)
_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   0.897
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     835
_refine_ls_number_reflns         12539
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      0.898
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0573
_refine_ls_shift/su_max          0.077
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.1841P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1784
_refine_ls_wR_factor_ref         0.1868
_reflns_number_gt                11754
_reflns_number_total             12539
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b508986g.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               7006374