Synthesis of Molecular Nanostructures by Multicomponent Condensation Reactions in a Ball Mill
Burçak Içli; Nicolas Christinat; Justus Tönnemann; Christian Schüttler; Rosario Scopelliti; Kay Severin; Journal of the American Chemical Society 131 (2009) 3154–3155; doi:10.1021/ja809279s

data_4104287
_publ_section_title
;
 Synthesis of Molecular Nanostructures by Multicomponent Condensation
 Reactions in a Ball Mill
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3154
_journal_page_last               3155
_journal_paper_doi               10.1021/ja809279s
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C87 H96 B6 N6 O12, 8(C2 H4 Cl2)'
_chemical_formula_sum            'C103 H128 B6 Cl16 N6 O12'
_chemical_formula_weight         2274.17
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   15.021(3)
_cell_length_b                   15.613(2)
_cell_length_c                   49.722(9)
_cell_measurement_reflns_used    60
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      11.823
_cell_measurement_theta_min      3.031
_cell_volume                     11661(3)
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs, 1990-2000)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0640
_diffrn_reflns_av_sigmaI/netI    0.0548
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            70710
_diffrn_reflns_theta_full        20.60
_diffrn_reflns_theta_max         20.60
_diffrn_reflns_theta_min         3.32
_exptl_absorpt_coefficient_mu    0.434
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10, G.M. Sheldrick, 2003'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4744
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.977
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.14(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1302
_refine_ls_number_reflns         11693
_refine_ls_number_restraints     888
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_gt           0.0739
_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^)+(0.0993P)^2^+43.9482P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1833
_refine_ls_wR_factor_ref         0.2010
_reflns_number_gt                9579
_reflns_number_total             11693
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja809279s_si_001.cif
_cod_data_source_block           cage_5
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               4104287