#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:40:49 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179511 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/08/4340808.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4340808
loop_
_publ_author_name
'Schweinfurth, David'
'Demeshko, Serhiy'
'Hohloch, Stephan'
'Steinmetz, Marc'
'Brandenburg, Jan Gerit'
'Dechert, Sebastian'
'Meyer, Franc'
'Grimme, Stefan'
'Sarkar, Biprajit'
_publ_section_title
;
 Spin Crossover in Fe(II) and Co(II) Complexes with the Same Click-Derived
 Tripodal Ligand.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8203
_journal_page_last               8212
_journal_paper_doi               10.1021/ic500264k
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C60 H60 Fe N20 2+, 2(B F4 -)'
_chemical_formula_sum            'C60 H60 B2 F8 Fe N20'
_chemical_formula_weight         1290.75
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                93.019(4)
_cell_angle_beta                 106.281(4)
_cell_angle_gamma                95.273(4)
_cell_formula_units_Z            1
_cell_length_a                   10.1366(5)
_cell_length_b                   11.4050(5)
_cell_length_c                   14.1339(7)
_cell_measurement_reflns_used    21546
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.756
_cell_measurement_theta_min      1.506
_cell_volume                     1556.56(13)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2002)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2012)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       ω
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0739
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21546
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.756
_diffrn_reflns_theta_min         1.506
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.323
_exptl_absorpt_correction_T_max  0.9547
_exptl_absorpt_correction_T_min  0.8853
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2002)'
_exptl_crystal_colour            'pale red-orange'
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_description       block
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.442
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         6606
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0455
_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/[σ²(Fo²)+(0.0809P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1231
_refine_ls_wR_factor_ref         0.1290
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5239
_reflns_number_total             6606
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic500264k_si_007.cif
_cod_data_source_block           h77rt
_cod_depositor_comments
'Adding full bibliography for 4340804--4340809.cif.'
_cod_database_code               4340808
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.855
_shelx_estimated_absorpt_t_max   0.953
_shelxl_version_number           2013-4
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Fe1 Fe 0.5000 0.5000 0.5000 0.03169(12) Uani 1 2 d S . P
N1 N 0.37456(16) 0.38703(14) 0.36980(12) 0.0402(3) Uani 1 1 d . . .
N11 N 0.63666(16) 0.38897(13) 0.48978(12) 0.0401(3) Uani 1 1 d . . .
N12 N 0.75778(19) 0.37234(18) 0.54829(15) 0.0595(5) Uani 1 1 d . . .
N13 N 0.7955(2) 0.27726(18) 0.50791(15) 0.0638(6) Uani 1 1 d . . .
N21 N 0.41550(16) 0.37630(13) 0.56856(12) 0.0397(3) Uani 1 1 d . . .
N22 N 0.44458(17) 0.34807(14) 0.66084(12) 0.0431(4) Uani 1 1 d . . .
N23 N 0.36878(16) 0.24517(13) 0.65859(12) 0.0413(3) Uani 1 1 d . . .
N31 N 0.26384(19) 0.33757(18) 0.12274(13) 0.0556(4) Uani 1 1 d . . .
N32 N 0.1666(2) 0.27224(19) 0.05447(14) 0.0592(5) Uani 1 1 d . . .
N33 N 0.05223(18) 0.26573(16) 0.08505(13) 0.0520(4) Uani 1 1 d . . .
C10 C 0.4691(3) 0.3154(3) 0.3346(2) 0.0757(8) Uani 1 1 d . . .
H10A H 0.4220 0.2371 0.3104 0.080 Uiso 1 1 calc R U .
H10B H 0.4923 0.3516 0.2799 0.080 Uiso 1 1 calc R U .
C11 C 0.5975(2) 0.30504(18) 0.41334(16) 0.0470(4) Uani 1 1 d . . .
C12 C 0.6999(2) 0.2332(2) 0.42462(18) 0.0589(6) Uani 1 1 d . . .
H12 H 0.7028 0.1677 0.3834 0.080 Uiso 1 1 calc R U .
C13 C 0.9290(4) 0.2332(4) 0.5538(3) 0.1195(17) Uani 1 1 d . . .
H13A H 0.9777 0.2235 0.5043 0.080 Uiso 1 1 calc R U .
H13B H 0.9121 0.1563 0.5769 0.080 Uiso 1 1 calc R U .
C14 C 1.0183(2) 0.3142(2) 0.63849(17) 0.0567(6) Uani 1 1 d . . .
C15 C 1.0364(3) 0.2840(3) 0.7325(2) 0.0777(8) Uani 1 1 d . . .
H15 H 0.9934 0.2131 0.7447 0.080 Uiso 1 1 calc R U .
C16 C 1.1211(4) 0.3613(4) 0.8109(2) 0.1060(13) Uani 1 1 d . . .
H16 H 1.1353 0.3416 0.8758 0.080 Uiso 1 1 calc R U .
C17 C 1.1811(4) 0.4633(4) 0.7924(4) 0.1083(13) Uani 1 1 d . . .
H17 H 1.2353 0.5150 0.8448 0.080 Uiso 1 1 calc R U .
C18 C 1.1648(4) 0.4918(3) 0.7007(5) 0.1117(15) Uani 1 1 d . . .
H18 H 1.2080 0.5628 0.6889 0.080 Uiso 1 1 calc R U .
C19 C 1.0847(3) 0.4171(3) 0.6235(3) 0.0842(9) Uani 1 1 d . . .
H19 H 1.0753 0.4372 0.5592 0.080 Uiso 1 1 calc R U .
C20 C 0.2696(3) 0.3121(2) 0.40221(17) 0.0617(6) Uani 1 1 d . . .
H20A H 0.1859 0.3507 0.3919 0.080 Uiso 1 1 calc R U .
H20B H 0.2466 0.2368 0.3628 0.080 Uiso 1 1 calc R U .
C21 C 0.3234(2) 0.29177(17) 0.50840(15) 0.0438(4) Uani 1 1 d . . .
C22 C 0.2931(2) 0.20652(17) 0.56555(15) 0.0457(4) Uani 1 1 d . . .
H22 H 0.2336 0.1371 0.5450 0.080 Uiso 1 1 calc R U .
C23 C 0.3867(2) 0.18459(18) 0.74900(16) 0.0485(5) Uani 1 1 d . . .
H23A H 0.3020 0.1347 0.7447 0.080 Uiso 1 1 calc R U .
H23B H 0.4030 0.2428 0.8047 0.080 Uiso 1 1 calc R U .
C24 C 0.5050(2) 0.10980(17) 0.76719(16) 0.0496(5) Uani 1 1 d . . .
C25 C 0.5294(3) 0.0434(2) 0.84790(19) 0.0678(7) Uani 1 1 d . . .
H25 H 0.4707 0.0430 0.8880 0.080 Uiso 1 1 calc R U .
C26 C 0.6406(4) -0.0226(2) 0.8696(2) 0.0831(9) Uani 1 1 d . . .
H26 H 0.6561 -0.0666 0.9245 0.080 Uiso 1 1 calc R U .
C27 C 0.7269(3) -0.0240(2) 0.8121(3) 0.0842(9) Uani 1 1 d . . .
H27 H 0.8013 -0.0686 0.8271 0.080 Uiso 1 1 calc R U .
C28 C 0.7039(4) 0.0404(3) 0.7322(3) 0.0960(11) Uani 1 1 d . . .
H28 H 0.7630 0.0400 0.6924 0.080 Uiso 1 1 calc R U .
C29 C 0.5930(3) 0.1067(3) 0.7094(3) 0.0800(8) Uani 1 1 d . . .
H29 H 0.5781 0.1498 0.6541 0.080 Uiso 1 1 calc R U .
C30 C 0.2980(2) 0.45134(19) 0.28525(15) 0.0500(5) Uani 1 1 d . . .
H30A H 0.2382 0.5004 0.3083 0.080 Uiso 1 1 calc R U .
H30B H 0.3645 0.5034 0.2650 0.080 Uiso 1 1 calc R U .
C31 C 0.2122(2) 0.37359(17) 0.19692(14) 0.0440(4) Uani 1 1 d . . .
C32 C 0.0770(2) 0.3271(2) 0.17316(16) 0.0514(5) Uani 1 1 d . . .
H32 H 0.0152 0.3360 0.2101 0.080 Uiso 1 1 calc R U .
C33 C -0.0729(3) 0.1903(2) 0.0274(2) 0.0695(7) Uani 1 1 d . . .
H33A H -0.0780 0.1161 0.0574 0.080 Uiso 1 1 calc R U .
H33B H -0.0664 0.1728 -0.0390 0.080 Uiso 1 1 calc R U .
C34 C -0.2024(2) 0.2467(2) 0.02131(17) 0.0556(5) Uani 1 1 d . . .
C35 C -0.2849(3) 0.2130(2) 0.0804(2) 0.0689(7) Uani 1 1 d . . .
H35 H -0.2580 0.1571 0.1256 0.080 Uiso 1 1 calc R U .
C36 C -0.4072(3) 0.2616(3) 0.0730(2) 0.0784(8) Uani 1 1 d . . .
H36 H -0.4618 0.2385 0.1132 0.080 Uiso 1 1 calc R U .
C37 C -0.4479(3) 0.3431(3) 0.0070(2) 0.0748(7) Uani 1 1 d . . .
H37 H -0.5311 0.3744 0.0013 0.080 Uiso 1 1 calc R U .
C38 C -0.3671(3) 0.3790(2) -0.0507(2) 0.0743(7) Uani 1 1 d . . .
H38 H -0.3944 0.4360 -0.0947 0.080 Uiso 1 1 calc R U .
C39 C -0.2448(3) 0.3313(2) -0.0443(2) 0.0683(7) Uani 1 1 d . . .
H39 H -0.1905 0.3561 -0.0843 0.080 Uiso 1 1 calc R U .
B1 B 0.9509(3) 0.0733(2) 0.3234(2) 0.0543(6) Uani 1 1 d . . .
F1 F 0.9404(3) 0.0231(2) 0.23134(14) 0.1196(8) Uani 1 1 d . . .
F2 F 1.07771(19) 0.05945(17) 0.38591(15) 0.0937(5) Uani 1 1 d . . .
F3 F 0.9375(2) 0.19238(14) 0.32083(15) 0.0888(5) Uani 1 1 d . . .
F4 F 0.8508(2) 0.02092(14) 0.36052(17) 0.0958(6) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N11 Fe1 N11 180.00(9) 2_666 .
N11 Fe1 N21 92.61(6) 2_666 .
N11 Fe1 N21 87.39(6) . .
N11 Fe1 N21 87.39(6) 2_666 2_666
N11 Fe1 N21 92.61(6) . 2_666
N21 Fe1 N21 180.0 . 2_666
N11 Fe1 N1 80.99(6) 2_666 2_666
N11 Fe1 N1 99.01(6) . 2_666
N21 Fe1 N1 99.00(6) . 2_666
N21 Fe1 N1 81.00(6) 2_666 2_666
N11 Fe1 N1 99.01(6) 2_666 .
N11 Fe1 N1 80.99(6) . .
N21 Fe1 N1 81.00(6) . .
N21 Fe1 N1 99.00(6) 2_666 .
N1 Fe1 N1 180.0 2_666 .
C10 N1 C20 112.0(2) . .
C10 N1 C30 108.09(18) . .
C20 N1 C30 107.35(16) . .
C10 N1 Fe1 107.40(12) . .
C20 N1 Fe1 106.89(12) . .
C30 N1 Fe1 115.21(12) . .
N12 N11 C11 109.96(16) . .
N12 N11 Fe1 132.77(13) . .
C11 N11 Fe1 116.96(13) . .
N11 N12 N13 105.98(17) . .
N12 N13 C12 111.60(18) . .
N12 N13 C13 121.0(2) . .
C12 N13 C13 127.4(2) . .
N22 N21 C21 110.09(15) . .
N22 N21 Fe1 133.46(12) . .
C21 N21 Fe1 115.57(13) . .
N21 N22 N23 105.90(15) . .
N22 N23 C22 111.54(15) . .
N22 N23 C23 119.37(16) . .
C22 N23 C23 128.74(16) . .
N32 N31 C31 109.38(18) . .
N31 N32 N33 107.00(17) . .
N32 N33 C32 110.61(17) . .
N32 N33 C33 120.0(2) . .
C32 N33 C33 129.2(2) . .
C11 C10 N1 112.15(19) . .
N11 C11 C12 107.57(18) . .
N11 C11 C10 117.80(18) . .
C12 C11 C10 134.3(2) . .
N13 C12 C11 104.89(19) . .
N13 C13 C14 112.6(2) . .
C19 C14 C15 118.8(3) . .
C19 C14 C13 121.3(3) . .
C15 C14 C13 119.9(3) . .
C14 C15 C16 118.9(3) . .
C17 C16 C15 119.9(3) . .
C18 C17 C16 121.0(4) . .
C17 C18 C19 119.9(3) . .
C14 C19 C18 121.4(3) . .
C21 C20 N1 110.52(17) . .
N21 C21 C22 107.76(17) . .
N21 C21 C20 118.10(17) . .
C22 C21 C20 133.92(18) . .
N23 C22 C21 104.70(17) . .
N23 C23 C24 112.73(17) . .
C29 C24 C25 117.8(2) . .
C29 C24 C23 123.5(2) . .
C25 C24 C23 118.7(2) . .
C24 C25 C26 120.5(3) . .
C27 C26 C25 120.8(3) . .
C26 C27 C28 119.4(3) . .
C27 C28 C29 120.5(3) . .
C24 C29 C28 121.0(3) . .
C31 C30 N1 114.85(17) . .
N31 C31 C32 107.72(18) . .
N31 C31 C30 122.13(18) . .
C32 C31 C30 130.15(19) . .
N33 C32 C31 105.29(19) . .
N33 C33 C34 112.6(2) . .
C35 C34 C39 118.2(2) . .
C35 C34 C33 120.1(2) . .
C39 C34 C33 121.6(2) . .
C34 C35 C36 120.6(3) . .
C37 C36 C35 120.3(3) . .
C36 C37 C38 120.1(3) . .
C37 C38 C39 120.4(3) . .
C38 C39 C34 120.5(3) . .
F1 B1 F2 109.3(2) . .
F1 B1 F4 111.0(2) . .
F2 B1 F4 108.5(2) . .
F1 B1 F3 110.8(2) . .
F2 B1 F3 108.6(2) . .
F4 B1 F3 108.6(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N11 1.9896(15) 2_666
Fe1 N11 1.9897(15) .
Fe1 N21 2.0125(15) .
Fe1 N21 2.0126(15) 2_666
Fe1 N1 2.1910(16) 2_666
Fe1 N1 2.1910(16) .
N1 C10 1.483(3) .
N1 C20 1.490(3) .
N1 C30 1.498(3) .
N11 N12 1.310(2) .
N11 C11 1.350(2) .
N12 N13 1.335(2) .
N13 C12 1.336(3) .
N13 C13 1.474(3) .
N21 N22 1.318(2) .
N21 C21 1.352(2) .
N22 N23 1.336(2) .
N23 C22 1.350(3) .
N23 C23 1.459(2) .
N31 N32 1.309(3) .
N31 C31 1.358(3) .
N32 N33 1.343(3) .
N33 C32 1.343(3) .
N33 C33 1.470(3) .
C10 C11 1.475(3) .
C11 C12 1.361(3) .
C13 C14 1.492(4) .
C14 C19 1.355(4) .
C14 C15 1.356(4) .
C15 C16 1.403(5) .
C16 C17 1.335(6) .
C17 C18 1.322(6) .
C18 C19 1.361(6) .
C20 C21 1.485(3) .
C21 C22 1.363(3) .
C23 C24 1.507(3) .
C24 C29 1.369(4) .
C24 C25 1.379(3) .
C25 C26 1.385(4) .
C26 C27 1.351(5) .
C27 C28 1.357(5) .
C28 C29 1.385(4) .
C30 C31 1.495(3) .
C31 C32 1.365(3) .
C33 C34 1.498(4) .
C34 C35 1.383(4) .
C34 C39 1.386(3) .
C35 C36 1.384(4) .
C36 C37 1.360(4) .
C37 C38 1.362(4) .
C38 C39 1.381(4) .
B1 F1 1.366(3) .
B1 F2 1.368(3) .
B1 F4 1.372(3) .
B1 F3 1.378(3) .
