Dihydroazulene-Buckminsterfullerene Conjugates
Marco Santella; Virginia Mazzanti; Martyn Jevric; Christian Richard Parker; Søren Lindbaek Broman; Andrew D. Bond; Mogens Brøndsted Nielsen; Journal of Organic Chemistry 77 (2012) 8922–8932; doi:10.1021/jo301306y

data_4027582
_publ_contact_author_address
;
University of Southern Denmark
Department of Physics and Chemistry
Campusvej 55
5230 Odense
Denmark
;
_publ_contact_author_email       adb@chem.sdu.dk
_publ_contact_author_fax         '+45 6615 8780'
_publ_contact_author_name        'Andrew D. Bond'
_publ_contact_author_phone       '+45 6650 2545'
_publ_section_title
;
 Dihydroazulene-Buckminsterfullerene Conjugates
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              8922
_journal_page_last               8932
_journal_paper_doi               10.1021/jo301306y
_journal_volume                  77
_journal_year                    2012
_chemical_formula_moiety         'C60, 2(C18 H11 I N2)'
_chemical_formula_sum            'C96 H22 I2 N4'
_chemical_formula_weight         1484.98
_chemical_name_common            MJ03
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   '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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.770(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.7913(15)
_cell_length_b                   10.5450(11)
_cell_length_c                   16.6502(17)
_cell_measurement_reflns_used    2198
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21.12
_cell_measurement_theta_min      2.75
_cell_volume                     2772.3(5)
_computing_cell_refinement       'SAINT v.7.68a (Bruker, 2010)'
_computing_data_collection       'APEX2 v2010.1-2 (Bruker, 2010)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL v.6.12 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker Nonius X8APEX-II CCD'
_diffrn_measurement_method       '\w and \f 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  0.0753
_diffrn_reflns_av_sigmaI/netI    0.1022
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13948
_diffrn_reflns_theta_full        25.17
_diffrn_reflns_theta_max         25.17
_diffrn_reflns_theta_min         3.53
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.202
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.779
_exptl_crystal_description       block
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.924
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         4836
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1036
_refine_ls_R_factor_gt           0.0613
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0570P)^2^+7.1436P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1300
_refine_ls_wR_factor_ref         0.1453
_reflns_number_gt                3229
_reflns_number_total             4836
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jo301306y_si_003.cif
_cod_data_source_block           2.C60
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4027582