#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/44/7034477.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_7034477
loop_
_publ_author_name
'Pimenta, Vanessa'
'Le, Quang Hoang Hanh'
'Clark, Lucy'
'Lhoste, Jérôme'
'Hémon-Ribaud, Annie'
'Leblanc, Marc'
'Grenèche, Jean-Marc'
'Dujardin, Gilles'
'Lightfoot, Philip'
'Maisonneuve, Vincent'
_publ_section_title
;
 New iron tetrazolate frameworks: synthesis, temperature effect, thermal
 behaviour, Mössbauer and magnetic studies.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7951
_journal_page_last               7959
_journal_paper_doi               10.1039/c5dt00281h
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C5 H11 F7 Fe5 N20 O3 1.5-,1.5(C2 H8 N 1+)'
_chemical_formula_sum            'C8 H23 F7 Fe5 N21.5 O3'
_chemical_formula_weight         880.73
_chemical_name_systematic        '[hdma]1.5(Fe5F7OwCOO)(Amtetraz)4)'
_space_group_IT_number           10
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2y'
_symmetry_space_group_name_H-M   'P 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-03-16 deposited with the CCDC.
2015-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 107.723(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   6.6118(6)
_cell_length_b                   12.4325(11)
_cell_length_c                   8.8075(7)
_cell_measurement_reflns_used    423
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.7
_cell_measurement_theta_min      2.4
_cell_volume                     689.63(10)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2007)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0808
_diffrn_reflns_av_sigmaI/netI    0.0469
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            16829
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    2.672
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_correction_T_min  0.852
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SHELX76; Sheldrick, 2008)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.121
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             438
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.911
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         1795
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0497P)²+1.0081P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1130
_reflns_number_gt                1355
_reflns_number_total             1795
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt00281h2.cif
_cod_data_source_block           '[hdma]1.5(Fe5F7OwCOO)(Amtetraz)4)'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3105 2015-03-04 15:46:00Z robertas 

 Adding full bibliography for 7034477--7034478.cif.
;
_cod_original_sg_symbol_H-M      'P 2/m'
_cod_original_formula_sum        'C8 H23 F7 Fe5 N21.50 O3'
_cod_database_code               7034477
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'-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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Fe1 Fe 0.5000 0.0000 1.0000 0.0157(2) Uani 1 4 d S
Fe2 Fe 1.0000 0.0000 1.0000 0.0141(2) Uani 1 4 d S
Fe3 Fe 0.5000 0.36653(6) 0.5000 0.0163(2) Uani 1 2 d S
Fe4 Fe 0.0000 0.5000 0.5000 0.0185(3) Uani 1 4 d S
F1 F 0.8042(5) 0.0000 1.1388(4) 0.0223(7) Uani 1 2 d S
F2 F 0.2183(4) 0.38055(18) 0.5425(3) 0.0273(5) Uani 1 1 d .
OW3 O 0.6061(6) 0.5000 0.6660(5) 0.0257(8) Uani 0.75 2 d SP
F3 F 0.6061(6) 0.5000 0.6660(5) 0.0257(8) Uani 0.25 2 d SP
OW4 O -0.0035(8) 0.5000 0.2577(5) 0.0447(12) Uani 0.75 2 d SP
F4 F -0.0035(8) 0.5000 0.2577(5) 0.0447(12) Uani 0.25 2 d SP
N1 N 0.7972(5) 0.1250(3) 0.8589(4) 0.0208(7) Uani 1 1 d .
N2 N 0.5890(5) 0.1212(3) 0.8501(4) 0.0209(7) Uani 1 1 d .
N3 N 0.4812(5) 0.1927(3) 0.7506(4) 0.0233(7) Uani 1 1 d .
N4 N 0.6162(5) 0.2471(3) 0.6892(4) 0.0203(7) Uani 1 1 d .
C1 C 0.8082(6) 0.2050(3) 0.7593(5) 0.0223(8) Uani 1 1 d .
N5 N 0.9897(6) 0.2360(4) 0.7306(6) 0.0520(14) Uani 1 1 d .
H5A H 0.9865 0.2863 0.6629 0.062 Uiso 1 1 calc R
H5B H 1.1080 0.2054 0.7802 0.062 Uiso 1 1 calc R
C4 C 0.176(2) 0.5000 0.2290(18) 0.043(3) Uani 0.50 2 d SP
C1A C 0.5000 0.4010(7) 1.0000 0.049(3) Uani 0.75 2 d SP
N1A N 0.437(2) 0.5000 0.9086(17) 0.035(3) Uani 0.375 2 d SP
C2A C -0.1875(16) 0.0000 0.5031(11) 0.046(3) Uani 0.75 2 d SP
N2A N -0.050(4) -0.0477(18) 0.460(2) 0.044(6) Uani 0.1875 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'
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
F1 Fe1 F1 180.0 . 3_657
F1 Fe1 N2 87.93(11) . .
F1 Fe1 N2 92.07(11) 3_657 .
F1 Fe1 N2 87.93(11) . 4
F1 Fe1 N2 92.07(11) 3_657 4
N2 Fe1 N2 86.54(17) . 4
F1 Fe1 N2 92.07(11) . 2_657
F1 Fe1 N2 87.93(11) 3_657 2_657
N2 Fe1 N2 93.46(17) . 2_657
N2 Fe1 N2 180.000(1) 4 2_657
F1 Fe1 N2 92.07(11) . 3_657
F1 Fe1 N2 87.93(11) 3_657 3_657
N2 Fe1 N2 179.999(1) . 3_657
N2 Fe1 N2 93.45(17) 4 3_657
N2 Fe1 N2 86.55(17) 2_657 3_657
F1 Fe2 F1 179.999(1) . 3_757
F1 Fe2 N1 87.07(11) . .
F1 Fe2 N1 92.93(11) 3_757 .
F1 Fe2 N1 87.07(11) . 4
F1 Fe2 N1 92.93(11) 3_757 4
N1 Fe2 N1 91.04(17) . 4
F1 Fe2 N1 92.93(11) . 2_757
F1 Fe2 N1 87.07(11) 3_757 2_757
N1 Fe2 N1 88.96(17) . 2_757
N1 Fe2 N1 180.0 4 2_757
F1 Fe2 N1 92.93(11) . 3_757
F1 Fe2 N1 87.07(11) 3_757 3_757
N1 Fe2 N1 180.00(12) . 3_757
N1 Fe2 N1 88.96(17) 4 3_757
N1 Fe2 N1 91.04(17) 2_757 3_757
F2 Fe3 F2 170.08(14) . 2_656
F2 Fe3 OW3 86.36(13) . .
F2 Fe3 OW3 86.09(12) 2_656 .
F2 Fe3 F3 86.10(12) . 3_666
F2 Fe3 F3 86.36(13) 2_656 3_666
OW3 Fe3 F3 80.94(16) . 3_666
F2 Fe3 OW3 86.10(12) . 3_666
F2 Fe3 OW3 86.36(13) 2_656 3_666
OW3 Fe3 OW3 80.94(16) . 3_666
F3 Fe3 OW3 0.0(2) 3_666 3_666
F2 Fe3 N4 94.02(11) . 2_656
F2 Fe3 N4 92.71(11) 2_656 2_656
OW3 Fe3 N4 173.15(12) . 2_656
F3 Fe3 N4 92.26(12) 3_666 2_656
OW3 Fe3 N4 92.26(12) 3_666 2_656
F2 Fe3 N4 92.71(11) . .
F2 Fe3 N4 94.02(11) 2_656 .
OW3 Fe3 N4 92.26(12) . .
F3 Fe3 N4 173.15(12) 3_666 .
OW3 Fe3 N4 173.15(12) 3_666 .
N4 Fe3 N4 94.55(17) 2_656 .
F2 Fe4 F2 180.0 4_565 2_556
F2 Fe4 F2 85.65(13) 4_565 3_566
F2 Fe4 F2 94.35(13) 2_556 3_566
F2 Fe4 F2 94.35(13) 4_565 .
F2 Fe4 F2 85.65(13) 2_556 .
F2 Fe4 F2 180.0 3_566 .
F2 Fe4 OW4 88.56(11) 4_565 .
F2 Fe4 OW4 91.44(11) 2_556 .
F2 Fe4 OW4 91.44(11) 3_566 .
F2 Fe4 OW4 88.56(11) . .
F2 Fe4 F4 91.44(11) 4_565 3_566
F2 Fe4 F4 88.56(11) 2_556 3_566
F2 Fe4 F4 88.56(11) 3_566 3_566
F2 Fe4 F4 91.44(11) . 3_566
OW4 Fe4 F4 179.999(1) . 3_566
F2 Fe4 OW4 91.44(11) 4_565 3_566
F2 Fe4 OW4 88.56(11) 2_556 3_566
F2 Fe4 OW4 88.56(11) 3_566 3_566
F2 Fe4 OW4 91.44(11) . 3_566
OW4 Fe4 OW4 179.999(1) . 3_566
F4 Fe4 OW4 0.0(3) 3_566 3_566
Fe1 F1 Fe2 109.69(14) . .
Fe3 F2 Fe4 132.53(12) . .
C4 OW3 Fe3 118.6(3) 3_666 3_666
C4 OW3 Fe3 118.6(3) 3_666 .
Fe3 OW3 Fe3 99.06(16) 3_666 .
C4 OW4 Fe4 117.9(7) . .
C1 N1 N2 104.2(3) . .
C1 N1 Fe2 139.0(3) . .
N2 N1 Fe2 116.5(2) . .
N3 N2 N1 110.7(3) . .
N3 N2 Fe1 133.0(3) . .
N1 N2 Fe1 116.2(2) . .
N2 N3 N4 108.5(3) . .
C1 N4 N3 105.6(3) . .
C1 N4 Fe3 132.9(3) . .
N3 N4 Fe3 121.4(2) . .
N4 C1 N1 111.0(3) . .
N4 C1 N5 124.9(4) . .
N1 C1 N5 124.0(4) . .
C1 N5 H5A 120.0 . .
C1 N5 H5B 120.0 . .
H5A N5 H5B 120.0 . .
OW4 C4 F3 132.0(12) . 3_666
OW4 C4 OW3 132.0(12) . 3_666
F3 C4 OW3 0.0(3) 3_666 3_666
N1A C1A N1A 65.1(10) . 3_667
C1A N1A C1A 114.9(10) 3_667 .
C1A N1A N1A 57.5(5) 3_667 3_667
C1A N1A N1A 57.5(5) . 3_667
N2A C2A N2A 57(2) . 4
N2A C2A N2A 58.6(16) . 3_556
N2A C2A N2A 29.2(14) 4 3_556
N2A C2A N2A 29.2(14) . 2_556
N2A C2A N2A 58.6(16) 4 2_556
N2A C2A N2A 43.0(17) 3_556 2_556
N2A N2A N2A 89.999(2) 2_556 4
N2A N2A C2A 103(4) 2_556 .
N2A N2A C2A 61.3(12) 4 .
N2A N2A N2A 55.7(15) 2_556 3_556
N2A N2A N2A 34.3(15) 4 3_556
C2A N2A N2A 74(2) . 3_556
N2A N2A C2A 48(3) 2_556 3_556
N2A N2A C2A 68.5(8) 4 3_556
C2A N2A C2A 121.4(16) . 3_556
N2A N2A C2A 47.2(16) 3_556 3_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 F1 2.011(3) .
Fe1 F1 2.011(3) 3_657
Fe1 N2 2.199(3) .
Fe1 N2 2.199(3) 4
Fe1 N2 2.199(3) 2_657
Fe1 N2 2.199(3) 3_657
Fe2 F1 2.033(3) .
Fe2 F1 2.033(3) 3_757
Fe2 N1 2.178(3) .
Fe2 N1 2.178(3) 4
Fe2 N1 2.178(3) 2_757
Fe2 N1 2.178(3) 3_757
Fe3 F2 2.016(2) .
Fe3 F2 2.016(2) 2_656
Fe3 OW3 2.181(3) .
Fe3 F3 2.181(3) 3_666
Fe3 OW3 2.181(3) 3_666
Fe3 N4 2.189(3) 2_656
Fe3 N4 2.189(3) .
Fe4 F2 2.025(2) 4_565
Fe4 F2 2.025(2) 2_556
Fe4 F2 2.025(2) 3_566
Fe4 F2 2.025(2) .
Fe4 OW4 2.127(5) .
Fe4 F4 2.127(5) 3_566
Fe4 OW4 2.127(5) 3_566
OW3 C4 1.459(16) 3_666
OW3 Fe3 2.181(3) 3_666
OW4 C4 1.284(16) .
N1 C1 1.343(5) .
N1 N2 1.356(4) .
N2 N3 1.298(4) .
N3 N4 1.357(4) .
N4 C1 1.338(5) .
C1 N5 1.355(5) .
N5 H5A 0.8600 .
N5 H5B 0.8600 .
C4 F3 1.459(16) 3_666
C4 OW3 1.459(16) 3_666
C1A N1A 1.460(11) .
C1A N1A 1.460(11) 3_667
N1A C1A 1.460(11) 3_667
N1A N1A 1.57(3) 3_667
C2A N2A 1.24(3) .
C2A N2A 1.24(3) 4
C2A N2A 1.62(3) 3_556
C2A N2A 1.62(3) 2_556
N2A N2A 0.81(3) 2_556
N2A N2A 1.19(5) 4
N2A N2A 1.44(4) 3_556
N2A C2A 1.62(3) 3_556
