#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:42:20 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180050 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/44/7034478.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_7034478
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         'C4 H12 F8 Fe5 N20 O2 1-,C2 H8 N 1+'
_chemical_formula_sum            'C6 H20 F8 Fe5 N21 O2'
_chemical_formula_weight         849.68
_chemical_name_systematic        '[hdma](Fe5F8Ow2(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                 110.439(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   6.6687(7)
_cell_length_b                   12.2450(10)
_cell_length_c                   9.0305(9)
_cell_measurement_reflns_used    2132
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.9
_cell_measurement_theta_min      2.4
_cell_volume                     690.99(12)
_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      150(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'ω scans'
_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  0.1477
_diffrn_reflns_av_sigmaI/netI    0.1027
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16982
_diffrn_reflns_theta_full        30.61
_diffrn_reflns_theta_max         30.61
_diffrn_reflns_theta_min         1.66
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.665
_exptl_absorpt_correction_T_max  0.923
_exptl_absorpt_correction_T_min  0.774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SHELX76; Sheldrick, 2008)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.042
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'small platelets'
_exptl_crystal_F_000             421
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.082
_refine_diff_density_min         -1.097
_refine_diff_density_rms         0.231
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         2206
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1502
_refine_ls_R_factor_gt           0.0852
_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)+(0.1354P)²+2.5109P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2212
_refine_ls_wR_factor_ref         0.2614
_reflns_number_gt                1269
_reflns_number_total             2206
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt00281h2.cif
_cod_data_source_block           '[hdma](Fe5F8Ow2(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_cell_volume        690.99(11)
_cod_original_sg_symbol_H-M      'P 2/m'
_cod_database_code               7034478
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 0.0000 0.0423(10) Uani 1 4 d S
Fe2 Fe 0.0000 0.0000 0.0000 0.0410(10) Uani 1 4 d S
Fe3 Fe 0.5000 0.36593(9) 0.5000 0.0232(4) Uani 1 2 d S
Fe4 Fe 0.0000 0.5000 0.5000 0.0274(6) Uani 1 4 d S
F1 F 0.190(2) 0.0000 -0.1361(7) 0.0397(18) Uani 1 2 d S
F2 F 0.2041(9) 0.3842(4) 0.5206(12) 0.065(2) Uani 1 1 d .
F3 F 0.587(2) 0.5000 0.6606(9) 0.044(2) Uani 0.50 2 d SP
OW3 O 0.587(2) 0.5000 0.6606(9) 0.044(2) Uani 0.50 2 d SP
F4 F 0.044(2) 0.5000 0.7241(12) 0.075(5) Uani 0.50 2 d SP
OW4 O 0.044(2) 0.5000 0.7241(12) 0.075(5) Uani 0.50 2 d SP
N1 N 0.209(2) 0.1248(7) 0.1406(12) 0.054(4) Uani 1 1 d .
N2 N 0.418(2) 0.1234(7) 0.1468(10) 0.059(4) Uani 1 1 d .
N3 N 0.522(2) 0.1964(7) 0.2489(11) 0.055(3) Uani 1 1 d .
N4 N 0.399(2) 0.2479(4) 0.3127(8) 0.046(2) Uani 1 1 d .
N5 N -0.0029(16) 0.2336(8) 0.2700(16) 0.071(4) Uani 1 1 d .
H5A H -0.1210 0.2011 0.2185 0.085 Uiso 1 1 calc R
H5B H -0.0007 0.2840 0.3370 0.085 Uiso 1 1 calc R
C1 C 0.204(2) 0.2018(8) 0.2425(12) 0.050(4) Uani 1 1 d .
C1A C 0.5000 0.401(3) 0.0000 0.044(7) Uiso 0.50 2 d SP
N1A N 0.457(8) 0.5000 -0.107(6) 0.036(10) Uiso 0.25 2 d SP
C2A C 0.185(3) 0.0000 -0.503(4) 0.027(4) Uiso 0.50 2 d SP
N2A N 0.003(11) 0.044(4) -0.446(6) 0.030(12) Uiso 0.125 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_655
F1 Fe1 N2 92.9(4) . 3_655
F1 Fe1 N2 87.1(4) 3_655 3_655
F1 Fe1 N2 87.1(4) . 4
F1 Fe1 N2 92.9(4) 3_655 4
N2 Fe1 N2 93.3(6) 3_655 4
F1 Fe1 N2 92.9(4) . 2_655
F1 Fe1 N2 87.1(4) 3_655 2_655
N2 Fe1 N2 86.7(6) 3_655 2_655
N2 Fe1 N2 180.0(3) 4 2_655
F1 Fe1 N2 87.1(4) . .
F1 Fe1 N2 92.9(4) 3_655 .
N2 Fe1 N2 179.999(1) 3_655 .
N2 Fe1 N2 86.7(6) 4 .
N2 Fe1 N2 93.3(6) 2_655 .
F1 Fe2 F1 179.999(1) . 3
F1 Fe2 N1 86.9(4) . .
F1 Fe2 N1 93.1(4) 3 .
F1 Fe2 N1 93.1(4) . 3
F1 Fe2 N1 86.9(4) 3 3
N1 Fe2 N1 180.000(1) . 3
F1 Fe2 N1 86.9(4) . 4
F1 Fe2 N1 93.1(4) 3 4
N1 Fe2 N1 90.2(6) . 4
N1 Fe2 N1 89.8(6) 3 4
F1 Fe2 N1 93.1(4) . 2
F1 Fe2 N1 86.9(4) 3 2
N1 Fe2 N1 89.8(6) . 2
N1 Fe2 N1 90.2(6) 3 2
N1 Fe2 N1 180.0(3) 4 2
F2 Fe3 F2 167.5(3) 2_656 .
F2 Fe3 F3 86.4(5) 2_656 .
F2 Fe3 F3 84.0(5) . .
F2 Fe3 OW3 84.0(5) 2_656 3_666
F2 Fe3 OW3 86.4(5) . 3_666
F3 Fe3 OW3 79.3(3) . 3_666
F2 Fe3 F3 84.0(5) 2_656 3_666
F2 Fe3 F3 86.4(5) . 3_666
F3 Fe3 F3 79.3(3) . 3_666
OW3 Fe3 F3 0.0(10) 3_666 3_666
F2 Fe3 N4 92.8(5) 2_656 .
F2 Fe3 N4 95.6(5) . .
F3 Fe3 N4 172.0(2) . .
OW3 Fe3 N4 92.7(2) 3_666 .
F3 Fe3 N4 92.7(2) 3_666 .
F2 Fe3 N4 95.6(5) 2_656 2_656
F2 Fe3 N4 92.8(5) . 2_656
F3 Fe3 N4 92.7(2) . 2_656
OW3 Fe3 N4 172.0(2) 3_666 2_656
F3 Fe3 N4 172.0(2) 3_666 2_656
N4 Fe3 N4 95.4(3) . 2_656
F2 Fe4 F2 94.6(3) . 4_565
F2 Fe4 F2 85.4(3) . 2_556
F2 Fe4 F2 180.0 4_565 2_556
F2 Fe4 F2 179.999(1) . 3_566
F2 Fe4 F2 85.4(3) 4_565 3_566
F2 Fe4 F2 94.6(3) 2_556 3_566
F2 Fe4 OW4 86.9(4) . 3_566
F2 Fe4 OW4 86.9(4) 4_565 3_566
F2 Fe4 OW4 93.1(4) 2_556 3_566
F2 Fe4 OW4 93.1(4) 3_566 3_566
F2 Fe4 F4 86.9(4) . 3_566
F2 Fe4 F4 86.9(4) 4_565 3_566
F2 Fe4 F4 93.1(4) 2_556 3_566
F2 Fe4 F4 93.1(4) 3_566 3_566
OW4 Fe4 F4 0.000(2) 3_566 3_566
F2 Fe4 F4 93.1(4) . .
F2 Fe4 F4 93.1(4) 4_565 .
F2 Fe4 F4 86.9(4) 2_556 .
F2 Fe4 F4 86.9(4) 3_566 .
OW4 Fe4 F4 180.000(4) 3_566 .
F4 Fe4 F4 180.000(4) 3_566 .
Fe1 F1 Fe2 110.7(3) . .
Fe4 F2 Fe3 137.5(3) . .
Fe3 F3 Fe3 100.7(3) 3_666 .
C1 N1 N2 104.4(11) . .
C1 N1 Fe2 138.3(12) . .
N2 N1 Fe2 116.9(8) . .
N3 N2 N1 107.7(12) . .
N3 N2 Fe1 135.8(12) . .
N1 N2 Fe1 116.5(7) . .
N2 N3 N4 112.2(13) . .
N3 N4 C1 103.8(7) . .
N3 N4 Fe3 126.4(9) . .
C1 N4 Fe3 129.5(11) . .
C1 N5 H5A 120.0 . .
C1 N5 H5B 120.0 . .
H5A N5 H5B 120.0 . .
N1 C1 N4 111.9(14) . .
N1 C1 N5 122.1(12) . .
N4 C1 N5 126.0(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 F1 2.001(11) .
Fe1 F1 2.001(11) 3_655
Fe1 N2 2.201(11) 3_655
Fe1 N2 2.201(11) 4
Fe1 N2 2.201(11) 2_655
Fe1 N2 2.201(11) .
Fe2 F1 2.051(12) .
Fe2 F1 2.051(12) 3
Fe2 N1 2.157(10) .
Fe2 N1 2.157(10) 3
Fe2 N1 2.157(10) 4
Fe2 N1 2.157(10) 2
Fe3 F2 2.058(6) 2_656
Fe3 F2 2.058(6) .
Fe3 F3 2.132(5) .
Fe3 OW3 2.132(5) 3_666
Fe3 F3 2.132(5) 3_666
Fe3 N4 2.146(6) .
Fe3 N4 2.146(6) 2_656
Fe4 F2 1.929(5) .
Fe4 F2 1.930(5) 4_565
Fe4 F2 1.930(5) 2_556
Fe4 F2 1.930(5) 3_566
Fe4 OW4 1.940(10) 3_566
Fe4 F4 1.940(10) 3_566
Fe4 F4 1.940(10) .
F3 Fe3 2.132(5) 3_666
N1 C1 1.325(14) .
N1 N2 1.377(16) .
N2 N3 1.299(11) .
N3 N4 1.319(17) .
N4 C1 1.352(17) .
N5 C1 1.537(19) .
N5 H5A 0.8600 .
N5 H5B 0.8600 .
