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#$Date: 2019-11-17 11:35:04 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229626 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/58/7045874.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_7045874
loop_
_publ_author_name
'Knoll, Christian'
'Müller, Danny'
'Seifried, Marco'
'Giester, Gerald'
'Welch, Jan M.'
'Artner, Werner'
'Hradil, Klaudia'
'Reissner, Michael'
'Weinberger, Peter'
_publ_section_title
;
 Cooperativity in spin crossover materials as ligand's responsibility -
 investigations of the Fe(ii) -
 1,3-bis((1H-tetrazol-1-yl)methyl)bicyclo[1.1.1]pentane system.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5553
_journal_page_last               5557
_journal_paper_doi               10.1039/c8dt00781k
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C4.5 H6 B0.33 F1.33 Fe0.17 N4'
_chemical_formula_weight         154.38
_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_Hall           '-P 3 2"c'
_space_group_name_H-M_alt        'P -3 c 1'
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/4
_audit_update_record
;
2017-07-26 deposited with the CCDC.
2018-03-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   11.3101(16)
_cell_length_b                   11.3101(16)
_cell_length_c                   19.393(4)
_cell_measurement_temperature    200(2)
_cell_volume                     2148.4(6)
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            16410
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.297
_diffrn_reflns_theta_min         3.603
_exptl_absorpt_coefficient_mu    0.439
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6781
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_F_000             948
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     108
_refine_ls_number_reflns         1781
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0506
_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)+(0.0550P)²+1.8861P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1324
_refine_ls_wR_factor_ref         0.1393
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1479
_reflns_number_total             1781
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt00781k2.cif
_cod_data_source_block           tu62_200k_sq
_cod_depositor_comments
'Adding full bibliography for 7045874--7045877.cif.'
_cod_original_cell_volume        2148.4(7)
_cod_original_formula_sum        'C4.50 H6 B0.33 F1.33 Fe0.17 N4'
_cod_database_code               7045874
_shelx_shelxl_version_number     2016/4
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
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 0.000000 0.000000 0.500000 0.0265(2) Uani 1 6 d S T P
N1 N 0.2925(2) 0.3658(2) 0.39591(10) 0.0340(5) Uani 1 1 d . . .
N2 N 0.1751(2) 0.3656(2) 0.38377(13) 0.0477(6) Uani 1 1 d . . .
N3 N 0.0780(2) 0.2530(2) 0.40888(12) 0.0431(5) Uani 1 1 d . . .
N4 N 0.1305(2) 0.1796(2) 0.43742(9) 0.0325(4) Uani 1 1 d . . .
C1 C 0.2631(2) 0.2514(2) 0.42828(12) 0.0342(5) Uani 1 1 d . . .
H1 H 0.327294 0.225448 0.442546 0.041 Uiso 1 1 calc R U .
C2 C 0.4235(3) 0.4795(2) 0.37222(13) 0.0411(6) Uani 1 1 d . . .
H2A H 0.499168 0.480507 0.398430 0.049 Uiso 1 1 calc R U .
H2B H 0.426093 0.567090 0.380469 0.049 Uiso 1 1 calc R U .
C3 C 0.4411(2) 0.4636(2) 0.29653(12) 0.0306(5) Uani 1 1 d . . .
C4 C 0.4514(2) 0.3451(2) 0.26304(13) 0.0359(5) Uani 1 1 d . . .
H4A H 0.534736 0.340749 0.273826 0.043 Uiso 1 1 calc R U .
H4B H 0.367250 0.254521 0.263804 0.043 Uiso 1 1 calc R U .
C5 C 0.5620(3) 0.5620(3) 0.250000 0.0354(7) Uani 1 2 d S T P
H5A H 0.569224 0.651173 0.239893 0.042 Uiso 0.5 1 calc R U P
H5B H 0.651174 0.569227 0.260107 0.042 Uiso 0.5 1 calc R U P
B1 B 0.666667 0.333333 0.4581(3) 0.0464(12) Uani 1 3 d S T P
F2 F 0.666667 0.333333 0.5270(6) 0.151(5) Uani 0.500(0) 3 d S T P
F3 F 0.666667 0.333333 0.3928(5) 0.219(9) Uani 0.500(0) 3 d S T P
F1A F 0.5455(8) 0.2710(12) 0.4833(5) 0.175(5) Uani 0.500(0) 1 d . . P
F1B F 0.5390(7) 0.2483(7) 0.4374(5) 0.118(3) Uani 0.500(0) 1 d . . P
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'
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'
N N 0.0061 0.0033 '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
N4 FE1 N4 87.84(7) . 8_556
N4 FE1 N4 92.16(7) . 2
N4 FE1 N4 180.0 8_556 2
N4 FE1 N4 87.84(7) . 9_556
N4 FE1 N4 92.16(7) 8_556 9_556
N4 FE1 N4 87.84(7) 2 9_556
N4 FE1 N4 92.16(7) . 3
N4 FE1 N4 87.84(7) 8_556 3
N4 FE1 N4 92.16(7) 2 3
N4 FE1 N4 180.0 9_556 3
N4 FE1 N4 180.0 . 7_556
N4 FE1 N4 92.16(7) 8_556 7_556
N4 FE1 N4 87.84(7) 2 7_556
N4 FE1 N4 92.16(7) 9_556 7_556
N4 FE1 N4 87.84(7) 3 7_556
C1 N1 N2 108.4(2) . .
C1 N1 C2 131.0(2) . .
N2 N1 C2 120.6(2) . .
N3 N2 N1 106.6(2) . .
N2 N3 N4 110.0(2) . .
C1 N4 N3 106.27(19) . .
C1 N4 FE1 132.97(16) . .
N3 N4 FE1 119.78(15) . .
N4 C1 N1 108.7(2) . .
N1 C2 C3 109.68(19) . .
C2 C3 C4 127.7(2) . 4
C2 C3 C4 125.8(2) . .
C4 C3 C4 87.88(19) 4 .
C2 C3 C5 127.20(19) . .
C4 C3 C5 87.54(16) 4 .
C4 C3 C5 87.48(16) . .
C2 C3 C3 178.8(2) . 4
C4 C3 C3 53.09(14) 4 4
C4 C3 C3 53.00(14) . 4
C5 C3 C3 53.16(11) . 4
C3 C4 C3 73.92(18) 4 .
C3 C5 C3 73.7(2) 4 .
F3 B1 F1A 112.4(5) . 3_665
F3 B1 F1A 112.4(6) . .
F1A B1 F1A 106.4(6) 3_665 .
F3 B1 F1A 112.4(5) . 2_655
F1A B1 F1A 106.4(6) 3_665 2_655
F1A B1 F1A 106.4(6) . 2_655
F3 B1 F1B 72.5(5) . 3_665
F1A B1 F1B 41.1(5) 3_665 3_665
F1A B1 F1B 114.7(8) . 3_665
F1A B1 F1B 132.8(8) 2_655 3_665
F3 B1 F1B 72.5(5) . .
F1A B1 F1B 132.8(8) 3_665 .
F1A B1 F1B 41.1(5) . .
F1A B1 F1B 114.7(8) 2_655 .
F1B B1 F1B 111.4(5) 3_665 .
F3 B1 F1B 72.5(5) . 2_655
F1A B1 F1B 114.7(8) 3_665 2_655
F1A B1 F1B 132.8(8) . 2_655
F1A B1 F1B 41.1(5) 2_655 2_655
F1B B1 F1B 111.4(5) 3_665 2_655
F1B B1 F1B 111.4(5) . 2_655
F3 B1 F2 180.0 . .
F1A B1 F2 67.6(5) 3_665 .
F1A B1 F2 67.6(5) . .
F1A B1 F2 67.6(5) 2_655 .
F1B B1 F2 107.5(5) 3_665 .
F1B B1 F2 107.5(5) . .
F1B B1 F2 107.5(5) 2_655 .
B1 F2 F1A 54.5(5) . 3_665
B1 F2 F1A 54.5(5) . .
F1A F2 F1A 89.6(6) 3_665 .
B1 F2 F1A 54.5(5) . 2_655
F1A F2 F1A 89.6(6) 3_665 2_655
F1A F2 F1A 89.7(6) . 2_655
B1 F3 F1B 55.9(4) . 3_665
B1 F3 F1B 55.9(4) . .
F1B F3 F1B 91.6(5) 3_665 .
B1 F3 F1B 55.9(4) . 2_655
F1B F3 F1B 91.6(5) 3_665 2_655
F1B F3 F1B 91.6(5) . 2_655
F1B F1A B1 72.5(8) . .
F1B F1A F2 128.5(11) . .
B1 F1A F2 57.9(6) . .
F1A F1B B1 66.5(7) . .
F1A F1B F3 116.7(10) . .
B1 F1B F3 51.6(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
FE1 N4 2.1858(19) .
FE1 N4 2.1858(19) 8_556
FE1 N4 2.1858(19) 2
FE1 N4 2.1858(19) 9_556
FE1 N4 2.1858(19) 3
FE1 N4 2.1858(19) 7_556
N1 C1 1.322(3) .
N1 N2 1.348(3) .
N1 C2 1.468(3) .
N2 N3 1.291(3) .
N3 N4 1.357(3) .
N4 C1 1.313(3) .
C2 C3 1.504(3) .
C3 C4 1.544(3) 4
C3 C4 1.546(3) .
C3 C5 1.549(3) .
C3 C3 1.858(5) 4
C4 C3 1.544(3) 4
C5 C3 1.549(3) 4
B1 F3 1.265(11) .
B1 F1A 1.284(8) 3_665
B1 F1A 1.284(8) .
B1 F1A 1.284(8) 2_655
B1 F1B 1.335(6) 3_665
B1 F1B 1.335(6) .
B1 F1B 1.335(6) 2_655
B1 F2 1.337(12) .
F2 F1A 1.458(11) 3_665
F2 F1A 1.458(11) .
F2 F1A 1.458(11) 2_655
F3 F1B 1.539(10) 3_665
F3 F1B 1.539(10) .
F3 F1B 1.539(10) 2_655
F1A F1B 0.920(11) .
