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_4108135
_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            'C14 H40 B2 N4 O9'
_chemical_formula_weight         430.12
_chemical_melting_point          422(1)
_chemical_name_common            '[(C3H7)4N][C(NH2)3]CO3[B(OH)3]2'
_chemical_name_systematic
; 
 ? 
;
_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                   16.024(6)
_cell_length_b                   13.854(5)
_cell_length_c                   11.651(4)
_cell_measurement_temperature    293(2)
_cell_volume                     2586.5(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0483
_diffrn_reflns_av_sigmaI/netI    0.0393
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17137
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.780476
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.105
_exptl_crystal_description       Block
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         3332
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.1214
_refine_ls_R_factor_gt           0.0688
_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^)+(0.1070P)^2^+1.1468P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2183
_refine_ls_wR_factor_ref         0.2621
_reflns_number_gt                1810
_reflns_number_total             3332
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja802425q-file002_2.cif
_cod_data_source_block           complex2
_cod_original_cell_volume        2586.5(15)
_cod_database_code               4108135