Steering Metallofullerene Electron Spin in Porous Metal-Organic Framework.
Feng, Yongqiang; Wang, Taishan; Li, Yongjian; Li, Jie; Wu, Jingyi; Wu, Bo; Jiang, Li; Wang, Chunru; Journal of the American Chemical Society 137 (2015) 15055–15060; doi:10.1021/jacs.5b10796

data_4129837
_publ_section_title
;
 Steering Metallofullerene Electron Spin in Porous Metal-Organic
 Framework.
;
_journal_issue                   47
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15055
_journal_page_last               15060
_journal_paper_doi               10.1021/jacs.5b10796
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         '0.13(C432 H240 O104 Zn32)'
_chemical_formula_sum            'C54 H30 O13 Zn4'
_chemical_formula_weight         1148.26
_space_group_crystal_system      trigonal
_space_group_IT_number           163
_space_group_name_Hall           '-P 3 2c'
_space_group_name_H-M_alt        'P -3 1 c'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-06-15
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            8
_cell_length_a                   37.166(5)
_cell_length_b                   37.166(5)
_cell_length_c                   30.111(6)
_cell_measurement_reflns_used    99646
_cell_measurement_temperature    293.1500
_cell_measurement_theta_max      31.3154
_cell_measurement_theta_min      1.0958
_cell_volume                     36020(10)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2014)'
_computing_structure_solution
;
'SHELXT (Sheldrick, 2014)'
;
_diffrn_ambient_temperature      293.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
scan:
	Number of images: 360
	           Slice: -110.0000 - 70.0000
	     Image width: 0.5000
	        Exp time: 30.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 45.1825
	          2theta: -19.8999
scan:
	Number of images: 360
	           Slice: -110.0000 - 70.0000
	     Image width: 0.5000
	        Exp time: 30.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 45.1825
	          2theta: -19.8999
scan:
	Number of images: 360
	           Slice: -110.0000 - 70.0000
	     Image width: 0.5000
	        Exp time: 30.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 45.1825
	          2theta: -19.8999
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0097
_diffrn_orient_matrix_UB_12      0.0133
_diffrn_orient_matrix_UB_13      -0.0263
_diffrn_orient_matrix_UB_21      0.0118
_diffrn_orient_matrix_UB_22      0.0287
_diffrn_orient_matrix_UB_23      0.0005
_diffrn_orient_matrix_UB_31      0.0304
_diffrn_orient_matrix_UB_32      -0.0125
_diffrn_orient_matrix_UB_33      0.0049
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1014
_diffrn_reflns_av_unetI/netI     0.0652
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            123302
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         0.633
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.544
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4497
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    0.423
_exptl_crystal_description       block
_exptl_crystal_F_000             4624
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.641
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     674
_refine_ls_number_reflns         21170
_refine_ls_number_restraints     1473
_refine_ls_restrained_S_all      1.761
_refine_ls_R_factor_all          0.1512
_refine_ls_R_factor_gt           0.1282
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3091
_refine_ls_wR_factor_ref         0.3226
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15337
_reflns_number_total             21170
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b10796_si_002.cif
_cod_data_source_block           1_a_sq
_cod_original_cell_volume        36021(13)
_cod_database_code               4129837
_diffrn_number_total             28077
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C1-C2 = C2-C3 = C3-C4 = C4-C5 = C5-C6 = C6-C1 = C7-C8 = C8-C9 = C9-C10
 1.39 with sigma of 0.01
 C10-C11 = C11-C12 = C12-C7 = C7-C8' = C8'-C9' = C9'-C10 = C10-C11'
 1.39 with sigma of 0.01
 C11'-C12' = C12'-C7 = C13-C14 = C14-C15 = C15-C16 = C16-C17 = C17-C18
 1.39 with sigma of 0.01
 C18-C13 = C13-C14' = C14'-C15' = C15'-C16 = C16-C17' = C17'-C18'
 1.39 with sigma of 0.01
 C18'-C13 = C19-C20 = C20-C21 = C21-C22 = C22-C23 = C23-C24 = C24-C19
 1.39 with sigma of 0.01
 C19-C20' = C20'-C21' = C21'-C22 = C22-C23' = C23'-C24' = C24'-C19
 1.39 with sigma of 0.01
 C28-C29 = C30-C31 = C31-C32 = C32-C33 = C33-C32' = C32'-C31' = C31'-C30
 1.39 with sigma of 0.01
 C35-C36 = C37-C38 = C38-C39 = C39-C40 = C40-C39' = C39'-C38' = C38'-C37
 1.39 with sigma of 0.01
 O1-C25 \\sim O2-C25 \\sim O1'-C25 \\sim O2'-C25 \\sim O3-C26 \\sim O4-C26
\\sim O3'-C26 \\sim O4'-C26
 with sigma of 0.01
 O3'-C26 \\sim O4'-C26 \\sim O5-C27 \\sim O6-C27 \\sim O5'-C27 \\sim O6'-C27
\\sim O7-C34 \\sim O7'-C34
 with sigma of 0.01
 O7'-C34 \\sim O8-C41 \\sim O8'-C41
 with sigma of 0.01
 O1-O2 \\sim O1'-O2' \\sim O3-O4 \\sim O3'-O4' \\sim O5-O6 \\sim O5'-O6'
 with sigma of 0.02
 O1-O2 \\sim O7-O7_$1 \\sim O7'-O7'_$1 \\sim O8-O8_$1 \\sim O8'-O8'_$1
 with sigma of 0.02
3. Restrained planarity
 C1, C2, C3, C4, C5, C6
 with sigma of 0.02
 C7, C8, C9, C10, C11, C12
 with sigma of 0.02
 C7, C8', C9', C10, C11', C12'
 with sigma of 0.02
 C13, C14, C15, C16, C17, C18
 with sigma of 0.02
 C13, C14', C15', C16, C17', C18'
 with sigma of 0.02
 C19, C20, C21, C22, C23, C24
 with sigma of 0.02
 C19, C20', C21', C22, C23', C24'
 with sigma of 0.02
 C30, C31, C32, C33
 with sigma of 0.02
 C30, C31', C32', C33
 with sigma of 0.02
 C37, C38, C39, C40
 with sigma of 0.02
 C37, C38', C39', C40
 with sigma of 0.02
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C10)
\\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C19) \\sim Ueq,
Uanis(C22) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27)
\\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C30) \\sim Ueq,
Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36)
\\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C41) \\sim Ueq,
Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C8') \\sim Ueq, Uanis(C9') \\sim Ueq, Uanis(C11') \\sim Ueq,
Uanis(C12') \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C17)
\\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq,
Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C32)
\\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C14') \\sim Ueq,
Uanis(C15') \\sim Ueq, Uanis(C17') \\sim Ueq, Uanis(C18') \\sim Ueq,
Uanis(C20') \\sim Ueq, Uanis(C21') \\sim Ueq, Uanis(C23') \\sim Ueq,
Uanis(C24') \\sim Ueq, Uanis(C31') \\sim Ueq, Uanis(C32') \\sim Ueq,
Uanis(C38') \\sim Ueq, Uanis(C39') \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(O8')
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
6. Others
 Sof(Zn3')=Sof(Zn4')=Sof(O3')=Sof(O4')=Sof(O5')=Sof(O6')=Sof(O7')=Sof(O8')=
 Sof(C14')=Sof(H14')=Sof(C15')=Sof(H15')=Sof(C17')=Sof(H17')=Sof(C18')=
 Sof(H18')=Sof(C20')=Sof(H20')=Sof(C21')=Sof(H21')=Sof(C23')=Sof(H23')=
 Sof(C24')=Sof(H24')=Sof(C31')=Sof(H31')=Sof(C32')=Sof(H32')=Sof(C38')=
 Sof(H38')=Sof(C39')=Sof(H39')=1-FVAR(1)
 Sof(Zn3)=Sof(Zn4)=Sof(O3)=Sof(O4)=Sof(O5)=Sof(O6)=Sof(O7)=Sof(O8)=Sof(C14)=
 Sof(H14)=Sof(C15)=Sof(H15)=Sof(C17)=Sof(H17)=Sof(C18)=Sof(H18)=Sof(C20)=
 Sof(H20)=Sof(C21)=Sof(H21)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(C31)=
 Sof(H31)=Sof(C32)=Sof(H32)=Sof(C38)=Sof(H38)=Sof(C39)=Sof(H39)=FVAR(1)
 Fixed Sof: Zn1(0.16667) Zn2(0.5) O1(0.5) O2(0.5) C8(0.5) H8(0.5) C9(0.5)
 H9(0.5) C11(0.5) H11(0.5) C12(0.5) H12(0.5) O1'(0.5) O2'(0.5) C8'(0.5)
 H8'(0.5) C9'(0.5) H9'(0.5) C11'(0.5) H11'(0.5) C12'(0.5) H12'(0.5)
 Fixed X: Zn1(0.33333)
 Fixed Y: Zn1(0.66667)
7.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C28(H28), C35(H35), C8(H8), C9(H9), C11(H11),
 C12(H12), C8'(H8'), C9'(H9'), C11'(H11'), C12'(H12'), C14(H14), C15(H15),
 C17(H17), C18(H18), C20(H20), C21(H21), C23(H23), C24(H24), C31(H31), C32(H32),
  C38(H38), C39(H39), C14'(H14'), C15'(H15'), C17'(H17'), C18'(H18'),
 C20'(H20'), C21'(H21'), C23'(H23'), C24'(H24'), C31'(H31'), C32'(H32'),
 C38'(H38'), C39'(H39')
;
_shelx_res_checksum              5637
_shelx_hkl_checksum              30886
_shelx_fab_checksum              20892
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'