The directional character of the piperazine double addition product, e{N(CH2CH2)2N}2C60, as a building block for forming crystalline fullerene polymers
Aghabali, Amineh; Jun, Sharon; Olmstead, Marilyn M.; Balch, Alan L.; CrystEngComm 20 (2018) 924–; doi:10.1039/C7CE02117H

data_7229960
_publ_section_title
;
 The directional character of the piperazine double addition product,
 e{N(CH2CH2)2N}2C60, as a building block for forming crystalline fullerene
 polymers
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              924
_journal_paper_doi               10.1039/C7CE02117H
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety
'2(C34 H8 N2), 2(I2), 2(C3 H3), 0.5(C S2), 0.5(C S2)'
_chemical_formula_sum            'C72 H19 I4 N4 S2'
_chemical_formula_weight         1511.63
_chemical_name_systematic        'e{N(CH2CH2)2N}2C60?3I2?CS2?C6H6 '
_chemical_properties_physical    Efflorescent
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-09-15 deposited with the CCDC.
2018-01-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.744(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.4566(7)
_cell_length_b                   10.6707(5)
_cell_length_c                   16.0942(7)
_cell_measurement_reflns_used    9966
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      43.948
_cell_measurement_theta_min      2.585
_cell_volume                     2390.99(19)
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_collection       'Apex 2 (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'XT (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker D8 with Photon 100 CMOS detector'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            61791
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         43.971
_diffrn_reflns_theta_min         2.584
_diffrn_source                   'Advanced Light Source, beamline 11.3.1'
_exptl_absorpt_coefficient_mu    3.428
_exptl_absorpt_correction_T_max  0.4458
_exptl_absorpt_correction_T_min  0.3944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2014)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.100
_exptl_crystal_description       block
_exptl_crystal_F_000             1446
_exptl_crystal_recrystallization_method
'diffusion of a CS2 solution of the fullerene with a solution of I2 in benzene'
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_refine_diff_density_max         3.182
_refine_diff_density_min         -2.267
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         14780
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0351P)^2^+6.1659P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.0927
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12163
_reflns_number_total             14780
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce02117h1.cif
_cod_data_source_block           aa96
_cod_depositor_comments
'Adding full bibliography for 7229960--7229961.cif.'
_cod_database_code               7229960
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.279
_shelx_estimated_absorpt_t_max   0.821
_shelx_res_checksum              32559