Rapid and efficient solvent-free synthesis of cyclophanes based on bipyridinium under mechanical ball milling
Xi, Hai-Tao; Zhao, Ting; Sun, Xiao-Qiang; Miao, Chun-Bao; Zong, Ting; Meng, Qi; RSC Adv. 3 (2013) 691–; doi:10.1039/C2RA22802E

data_7238793
_publ_section_title
;
 Rapid and efficient solvent-free synthesis of cyclophanes based on
 bipyridinium under mechanical ball milling
;
_journal_issue                   3
_journal_name_full               'RSC Adv.'
_journal_page_first              691
_journal_paper_doi               10.1039/C2RA22802E
_journal_volume                  3
_journal_year                    2013
_chemical_formula_sum            'C37 H34 F24 N4 O P4'
_chemical_formula_weight         1130.56
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2011-01-29 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.130(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.692(3)
_cell_length_b                   20.230(7)
_cell_length_c                   14.097(5)
_cell_measurement_temperature    296(2)
_cell_volume                     2187.9(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1073
_diffrn_reflns_av_sigmaI/netI    0.1324
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13065
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    0.314
_exptl_crystal_density_diffrn    1.716
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1136
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         4309
_refine_ls_number_restraints     665
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.2205
_refine_ls_R_factor_gt           0.0744
_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^)+(0.0200P)^2^+4.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1323
_refine_ls_wR_factor_ref         0.1699
_reflns_number_gt                1527
_reflns_number_total             4309
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ra22802e.txt
_cod_data_source_block           x
_cod_database_code               7238793