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_4111864
_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            'C44 H124 N16 O28'
_chemical_formula_weight         1325.59
_chemical_name_systematic
; 
 4(Et4N+)8[C(NH2)3+]3[(CO3)2-]3[(C2O4)2-]2(H2O) 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                   35.9775(16)
_cell_length_b                   14.2730(6)
_cell_length_c                   11.9582(5)
_cell_measurement_temperature    293(2)
_cell_volume                     6140.6(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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0461
_diffrn_reflns_av_sigmaI/netI    0.0314
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            34870
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         1.13
_exptl_absorpt_coefficient_mu    0.118
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       block
_exptl_crystal_F_000             2896
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.713
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       0.0080(13)
_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   1.939
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         6291
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.940
_refine_ls_R_factor_all          0.1410
_refine_ls_R_factor_gt           0.1013
_refine_ls_shift/su_max          6.404
_refine_ls_shift/su_mean         0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0859P)^2^+0.1168P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2789
_refine_ls_wR_factor_ref         0.2935
_reflns_number_gt                3623
_reflns_number_total             6291
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja050221asi20050113_021602_1.cif
_cod_data_source_block           oxe4g(2)
_cod_database_code               4111864