Inclusion of unique four-clawed crown-like nitrate–water cluster [(NO3)6(H2O)6]6− anions into the inter-spaces of a 3D H–bonded cationic net formed by a cationic calix[4]arene
Liu, Lei-Lei; Ren, Zhi-Gang; Wan, Li-Min; Ding, Hong-Ye; Lang, Jian-Ping; CrystEngComm 13 (2011) 5718–; doi:10.1039/c1ce05377a

data_7206509
_publ_section_title
;
 Inclusion of unique four-clawed crown-like nitrate--water cluster
 [(NO3)6(H2O)6]6&#x2212; anions into the inter-spaces of a 3D H--bonded
 cationic net formed by a cationic calix[4]arene
;
_journal_issue                   19
_journal_name_full               CrystEngComm
_journal_page_first              5718
_journal_paper_doi               10.1039/c1ce05377a
_journal_volume                  13
_journal_year                    2011
_chemical_formula_moiety         'C40 H55 N4 O4, 3(N O3), 2(C2 H3 N), 3(H2 O)'
_chemical_formula_sum            'C44 H67 N9 O16'
_chemical_formula_weight         978.07
_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                92.13(3)
_cell_angle_beta                 105.50(3)
_cell_angle_gamma                101.33(3)
_cell_formula_units_Z            2
_cell_length_a                   13.498(3)
_cell_length_b                   13.840(3)
_cell_length_c                   13.990(3)
_cell_measurement_reflns_used    9101
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.5165
_cell_measurement_theta_min      3.0100
_cell_volume                     2458.2(11)
_computing_cell_refinement       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_collection       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_reduction
'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_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  0.0496
_diffrn_reflns_av_sigmaI/netI    0.0676
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20473
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.01
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_T_max  0.9800
_exptl_absorpt_correction_T_min  0.9606
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Jacobson, R. (1998) Private communication to Rigaku Corp.'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.640
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     659
_refine_ls_number_reflns         8593
_refine_ls_number_restraints     321
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1181
_refine_ls_R_factor_gt           0.0716
_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^)+(0.1056P)^2^+0.3716P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1772
_refine_ls_wR_factor_ref         0.2045
_reflns_number_gt                5423
_reflns_number_total             8593
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1ce05377a.txt
_cod_data_source_block           2
_cod_original_cell_volume        2458.1(9)
_cod_database_code               7206509