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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/7/04/58/7045877.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_7045877
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            'C27 H36 Cl2 Fe N24 O8'
_chemical_formula_weight         951.55
_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            2
_cell_length_a                   11.2861(3)
_cell_length_b                   11.2861(3)
_cell_length_c                   19.6585(6)
_cell_measurement_temperature    250(2)
_cell_volume                     2168.55(11)
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_diffrn_ambient_temperature      250(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  0.0429
_diffrn_reflns_av_unetI/netI     0.0146
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            51862
_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         30.531
_diffrn_reflns_theta_min         3.611
_exptl_absorpt_coefficient_mu    0.545
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6916
_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    1.457
_exptl_crystal_F_000             980
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     108
_refine_ls_number_reflns         2219
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0446
_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)+(0.0631P)²+1.2790P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1301
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1792
_reflns_number_total             2219
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt00781k2.cif
_cod_data_source_block           tu65_250k_sq
_cod_depositor_comments
'Adding full bibliography for 7045874--7045877.cif.'
_cod_original_cell_volume        2168.55(13)
_cod_database_code               7045877
_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
FE Fe 0.000000 0.000000 0.500000 0.02460(15) Uani 1 6 d S T P
N1 N 0.28229(16) 0.36562(15) 0.39355(8) 0.0351(3) Uani 1 1 d . . .
N2 N 0.16272(19) 0.35925(18) 0.38003(10) 0.0474(4) Uani 1 1 d . . .
N3 N 0.06810(18) 0.24813(18) 0.40670(9) 0.0436(4) Uani 1 1 d . . .
N4 N 0.12383(15) 0.18039(15) 0.43781(7) 0.0322(3) Uani 1 1 d . . .
C1 C 0.25725(19) 0.25583(19) 0.42856(9) 0.0369(4) Uani 1 1 d . . .
H1 H 0.323266 0.234808 0.444286 0.044 Uiso 1 1 calc R U .
C2 C 0.4121(2) 0.47967(18) 0.36879(10) 0.0432(5) Uani 1 1 d . . .
H2A H 0.487962 0.485683 0.395742 0.052 Uiso 1 1 calc R U .
H2B H 0.411586 0.565745 0.374135 0.052 Uiso 1 1 calc R U .
C3 C 0.43226(17) 0.45882(16) 0.29536(9) 0.0316(3) Uani 1 1 d . . .
C4 C 0.4430(2) 0.33814(18) 0.26537(10) 0.0386(4) Uani 1 1 d . . .
H4A H 0.359124 0.248688 0.266221 0.046 Uiso 1 1 calc R U .
H4B H 0.524792 0.333722 0.277889 0.046 Uiso 1 1 calc R U .
C5 C 0.5551(2) 0.5551(2) 0.250000 0.0368(5) Uani 1 2 d S T P
H5A H 0.643086 0.562746 0.261625 0.044 Uiso 0.5 1 calc R U P
H5B H 0.562749 0.643087 0.238376 0.044 Uiso 0.5 1 calc R U P
CL Cl 0.666667 0.333333 0.45933(5) 0.0490(2) Uani 1 3 d S T P
O2 O 0.666667 0.333333 0.5251(7) 0.217(10) Uani 0.500(0) 3 d S T P
O3 O 0.666667 0.333333 0.3944(5) 0.200(9) Uani 0.500(0) 3 d S T P
O1A O 0.5445(8) 0.2843(14) 0.4894(5) 0.201(6) Uani 0.500(0) 1 d . . P
O1B O 0.5371(8) 0.2398(8) 0.4354(5) 0.160(4) 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
N4 FE N4 180.0 8_556 2
N4 FE N4 91.59(6) 8_556 9_556
N4 FE N4 88.41(6) 2 9_556
N4 FE N4 88.41(6) 8_556 3
N4 FE N4 91.59(6) 2 3
N4 FE N4 180.00(6) 9_556 3
N4 FE N4 91.59(6) 8_556 7_556
N4 FE N4 88.41(6) 2 7_556
N4 FE N4 91.59(6) 9_556 7_556
N4 FE N4 88.41(6) 3 7_556
N4 FE N4 88.41(6) 8_556 .
N4 FE N4 91.59(6) 2 .
N4 FE N4 88.41(6) 9_556 .
N4 FE N4 91.59(6) 3 .
N4 FE N4 180.0 7_556 .
C1 N1 N2 108.41(15) . .
C1 N1 C2 130.41(18) . .
N2 N1 C2 121.16(16) . .
N3 N2 N1 107.12(15) . .
N2 N3 N4 109.97(16) . .
C1 N4 N3 105.99(14) . .
C1 N4 FE 132.20(12) . .
N3 N4 FE 121.25(12) . .
N1 C1 N4 108.50(16) . .
N1 C1 H1 125.7 . .
N4 C1 H1 125.7 . .
N1 C2 C3 110.20(15) . .
N1 C2 H2A 109.6 . .
C3 C2 H2A 109.6 . .
N1 C2 H2B 109.6 . .
C3 C2 H2B 109.6 . .
H2A C2 H2B 108.1 . .
C2 C3 C4 126.29(16) . .
C2 C3 C5 126.77(14) . .
C4 C3 C5 87.78(12) . .
C2 C3 C4 127.71(16) . 4
C4 C3 C4 87.49(15) . 4
C5 C3 C4 87.63(12) . 4
C2 C3 C3 179.3(2) . 4
C4 C3 C3 53.18(11) . 4
C5 C3 C3 53.08(8) . 4
C4 C3 C3 52.97(10) 4 4
C3 C4 C3 73.86(14) . 4
C3 C4 H4A 116.1 . .
C3 C4 H4A 116.1 4 .
C3 C4 H4B 116.1 . .
C3 C4 H4B 116.1 4 .
H4A C4 H4B 113.1 . .
C3 C5 C3 73.84(17) . 4
C3 C5 H5A 116.1 . .
C3 C5 H5A 116.1 4 .
C3 C5 H5B 116.1 . .
C3 C5 H5B 116.1 4 .
H5A C5 H5B 113.1 . .
O3 CL O2 180.0 . .
O3 CL O1A 116.2(4) . .
O2 CL O1A 63.8(4) . .
O3 CL O1A 116.2(4) . 2_655
O2 CL O1A 63.8(4) . 2_655
O1A CL O1A 102.0(5) . 2_655
O3 CL O1A 116.2(4) . 3_665
O2 CL O1A 63.8(4) . 3_665
O1A CL O1A 102.0(5) . 3_665
O1A CL O1A 102.0(5) 2_655 3_665
O3 CL O1B 70.2(5) . 2_655
O2 CL O1B 109.8(5) . 2_655
O1A CL O1B 143.6(7) . 2_655
O1A CL O1B 50.3(5) 2_655 2_655
O1A CL O1B 106.5(8) 3_665 2_655
O3 CL O1B 70.2(5) . .
O2 CL O1B 109.8(5) . .
O1A CL O1B 50.3(5) . .
O1A CL O1B 106.5(8) 2_655 .
O1A CL O1B 143.6(7) 3_665 .
O1B CL O1B 109.1(5) 2_655 .
O3 CL O1B 70.2(5) . 3_665
O2 CL O1B 109.8(5) . 3_665
O1A CL O1B 106.5(8) . 3_665
O1A CL O1B 143.6(7) 2_655 3_665
O1A CL O1B 50.3(5) 3_665 3_665
O1B CL O1B 109.1(5) 2_655 3_665
O1B CL O1B 109.1(5) . 3_665
CL O2 O1A 59.7(5) . .
CL O2 O1A 59.7(5) . 2_655
O1A O2 O1A 96.8(7) . 2_655
CL O2 O1A 59.7(5) . 3_665
O1A O2 O1A 96.8(7) . 3_665
O1A O2 O1A 96.8(7) 2_655 3_665
CL O3 O1B 58.4(4) . 2_655
CL O3 O1B 58.4(4) . .
O1B O3 O1B 95.0(6) 2_655 .
CL O3 O1B 58.4(4) . 3_665
O1B O3 O1B 95.0(6) 2_655 3_665
O1B O3 O1B 95.0(6) . 3_665
O1B O1A CL 67.1(6) . .
O1B O1A O2 118.5(10) . .
CL O1A O2 56.5(6) . .
O1A O1B CL 62.6(5) . .
O1A O1B O3 110.2(8) . .
CL O1B O3 51.4(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
FE N4 2.1788(14) 8_556
FE N4 2.1788(14) 2
FE N4 2.1788(14) 9_556
FE N4 2.1788(14) 3
FE N4 2.1788(14) 7_556
FE N4 2.1788(14) .
N1 C1 1.319(2) .
N1 N2 1.342(2) .
N1 C2 1.468(2) .
N2 N3 1.284(2) .
N3 N4 1.355(2) .
N4 C1 1.320(2) .
C1 H1 0.9400 .
C2 C3 1.498(3) .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C3 C4 1.544(2) .
C3 C5 1.546(2) .
C3 C4 1.548(2) 4
C3 C3 1.858(3) 4
C4 C3 1.548(3) 4
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C5 C3 1.546(2) 4
C5 H5A 0.9800 .
C5 H5B 0.9800 .
CL O3 1.276(10) .
CL O2 1.293(13) .
CL O1A 1.339(7) .
CL O1A 1.339(7) 2_655
CL O1A 1.339(7) 3_665
CL O1B 1.389(6) 2_655
CL O1B 1.389(6) .
CL O1B 1.389(6) 3_665
O2 O1A 1.392(10) .
O2 O1A 1.392(10) 2_655
O2 O1A 1.392(10) 3_665
O3 O1B 1.535(11) 2_655
O3 O1B 1.535(11) .
O3 O1B 1.535(11) 3_665
O1A O1B 1.160(11) .
