Hydrogen-Bonded Anionic Rosette Networks Assembled with Guanidinium and C3-Symmetric Oxoanion Building Blocks
Chi-Keung Lam; Feng Xue; Jie-Peng Zhang; Xiao-Ming Chen; Thomas C. W. Mak; Journal of the American Chemical Society 127 (2005) 11536–11537; doi:10.1021/ja050221a

data_4111865
_publ_section_title
;
 Hydrogen-Bonded Anionic Rosette Networks Assembled with Guanidinium and
 C3-Symmetric Oxoanion Building Blocks
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11536
_journal_page_last               11537
_journal_paper_doi               10.1021/ja050221a
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C26 H60 N5 O12'
_chemical_formula_weight         634.79
_chemical_name_systematic
; 
 2(Et4N+)[C(NH2)3+][1,3,5-C6H3(COO-)3]6(H2O) 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                   12.0977(9)
_cell_length_b                   20.9279(15)
_cell_length_c                   14.5969(10)
_cell_measurement_temperature    123
_cell_volume                     3695.6(5)
_computing_cell_refinement       'SAINT-PLUS, Ver. 5.0, Bruker AXS, 1997.'
_computing_data_collection       'SMART for Windows NT, Bruker AXS, 1997.'
_computing_data_reduction        'SAINT-PLUS, Ver. 5.0, Bruker AXS, 1997.'
_computing_molecular_graphics    'XP-Interactive Molecular Graphics, Ver. 5.1'
_computing_publication_material  'SHELXTL-Bruker AXS, 1998.'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART CCD 1K'
_diffrn_measurement_method       'omega scan'
_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  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0204
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21958
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_description       block
_exptl_crystal_F_000             1388
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.41
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.173
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         3261
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0685P)^2^+1.2940P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1257
_refine_ls_wR_factor_ref         0.1316
_reflns_number_gt                2766
_reflns_number_total             3261
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja050221asi20050113_021602_2.cif
_cod_data_source_block           CK47-150
_cod_database_code               4111865