Designed Supramolecular Assembly of Hydrogen-Bonded Anionic Rosette Layers
Jie Han; Chung-Wah Yau; Chi-Keung Lam; Thomas C. W. Mak; Journal of the American Chemical Society 130 (2008) 10315–10326; doi:10.1021/ja802425q

data_4108138
_publ_section_title
;
 Designed Supramolecular Assembly of Hydrogen-Bonded Anionic Rosette
 Layers
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10315
_journal_page_last               10326
_journal_paper_doi               10.1021/ja802425q
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C29 H42 N4 O8'
_chemical_formula_weight         574.67
_chemical_name_common            '[(C3H7)4N][C(NH2)3][(C6H3)2(COOH)2(COO)2]'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 101.315(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.2393(17)
_cell_length_b                   15.769(2)
_cell_length_c                   16.204(2)
_cell_measurement_temperature    293(2)
_cell_volume                     3066.6(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0419
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            21199
_diffrn_reflns_theta_full        28.35
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.780959
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.194
_refine_diff_density_min         -0.197
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         7634
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0979
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0542P)^2^+0.7218P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1083
_refine_ls_wR_factor_ref         0.1373
_reflns_number_gt                4415
_reflns_number_total             7634
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja802425q-file002_5.cif
_cod_data_source_block           complex5
_cod_original_cell_volume        3066.7(7)
_cod_database_code               4108138