Complexation of Sc3N@C80 Endohedral Fullerene with Cyclic Zn-Bisporphyrins: Solid State and Solution Studies
Laura P. Hernández-Eguía; Eduardo C. Escudero-Adán; Julio R. Pinzón; Luis Echegoyen; Pablo Ballester; Journal of Organic Chemistry 76 (2011) 3258–3265; doi:10.1021/jo200154d

data_4026248
_publ_section_title
;
 Complexation of Sc3N@C80 Endohedral Fullerene with Cyclic
 Zn-Bisporphyrins: Solid State and Solution Studies
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              3258
_journal_page_last               3265
_journal_paper_doi               10.1021/jo200154d
_journal_volume                  76
_journal_year                    2011
_chemical_formula_sum            'C118 H99 N10 O6 Zn2'
_chemical_formula_weight         1883.81
_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                 94.558(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.803(8)
_cell_length_b                   23.382(13)
_cell_length_c                   33.72(3)
_cell_measurement_reflns_used    706
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      14.51
_cell_measurement_theta_min      2.46
_cell_volume                     10062(12)
_computing_cell_refinement       'Bruker APEX2 v2009.1-0'
_computing_data_collection       'Bruker APEX2 v2009.1-0'
_computing_data_reduction        'Bruker SAINT V7.60A'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_detector_type            '4K CCD area detector APEX II'
_diffrn_measured_fraction_theta_full 0.883
_diffrn_measured_fraction_theta_max 0.883
_diffrn_measurement_device_type  'Kappa 4-axis goniometer bruker-nonius'
_diffrn_measurement_method
;
 Fullsphere data collection, phi and omega scans
;
_diffrn_measurement_specimen_support
'magnetic support whith 10 micron nylon fiber cryoloop'
_diffrn_radiation_monochromator  'Multilayer Montel 200 mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2415
_diffrn_reflns_av_sigmaI/netI    0.2366
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            22265
_diffrn_reflns_theta_full        19.05
_diffrn_reflns_theta_max         19.05
_diffrn_reflns_theta_min         1.06
_diffrn_source                   'rotating anode X-ray tube'
_diffrn_source_current           70
_diffrn_source_power             50
_diffrn_source_size              '3 mm x 0.3 mm fine focus'
_diffrn_source_type              'Bruker-Nonius FR 591'
_exptl_absorpt_coefficient_mu    0.538
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 SADABS Version 2008/1 Bruker-Nonius
 Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_description       Needle
_exptl_crystal_F_000             3940
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.699
_refine_diff_density_min         -0.713
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.221
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1258
_refine_ls_number_reflns         7206
_refine_ls_number_restraints     1313
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.2318
_refine_ls_R_factor_gt           0.0990
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2227
_refine_ls_wR_factor_ref         0.2810
_reflns_number_gt                3072
_reflns_number_total             7206
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo200154d_si_004.cif
_cod_data_source_block           lph244tmeda_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_diffrn_measurement_specimen_suppport' was replaced with
'_diffrn_measurement_specimen_support' as specified in the
replacement file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
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_cod_original_cell_volume        10062(11)
_cod_database_code               4026248