#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/34/4513493.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_4513493
loop_
_publ_author_name
'Pimenta, Vanessa'
'Lhoste, Jérôme'
'Hémon-Ribaud, Annie'
'Leblanc, Marc'
'Grenèche, Jean-Marc'
'Jouffret, Laurent'
'Martel, Arnaud'
'Dujardin, Gilles'
'Maisonneuve, Vincent'
_publ_section_title
;
 Evidence of New Fluorinated Coordination Compounds in the Composition
 Space Diagram of FeF3/ZnF2--Hamtetraz-HFaqSystem
;
_journal_issue                   9
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              4248
_journal_paper_doi               10.1021/acs.cgd.5b00530
_journal_volume                  15
_journal_year                    2015
_chemical_formula_moiety         'C4 H8 F5 N20 Zn4, C N, 2(C0.50)'
_chemical_formula_sum            'C6 H8 F5 N21 Zn4'
_chemical_formula_weight         730.89
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.579(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   6.5576(4)
_cell_length_b                   9.7150(6)
_cell_length_c                   8.6358(6)
_cell_measurement_reflns_used    4152
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      52.12
_cell_measurement_theta_min      6.34
_cell_volume                     550.13(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1227
_diffrn_reflns_av_sigmaI/netI    0.0463
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            24338
_diffrn_reflns_theta_full        30.56
_diffrn_reflns_theta_max         30.56
_diffrn_reflns_theta_min         2.10
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.396
_exptl_absorpt_correction_T_max  0.876
_exptl_absorpt_correction_T_min  0.628
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SHELX76; Sheldrick, 2008)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    2.206
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             356
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         5.166
_refine_diff_density_min         -1.810
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         1791
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0557
_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)+(0.0578P)²+5.5798P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1358
_refine_ls_wR_factor_ref         0.1467
_reflns_number_gt                1570
_reflns_number_total             1791
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg5b00530_si_006.cif
_cod_data_source_block           Zn4F5amtetraz4hdma
_cod_depositor_comments
'Adding full bibliography for 4513493--4513496.cif.'
_cod_original_sg_symbol_H-M      'P 2/m'
_cod_database_code               4513493
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
Zn1 Zn 0.29709(13) 0.5000 0.59708(10) 0.0085(2) Uani 1 2 d S
Zn2 Zn 0.0000 0.0000 1.0000 0.0094(3) Uani 1 4 d S
Zn3 Zn 0.5000 0.0000 1.0000 0.0154(3) Uani 1 4 d S
F1 F 0.2579(7) 0.0000 1.1383(5) 0.0112(9) Uani 1 2 d S
F2 F 0.3852(7) 0.5000 0.3822(6) 0.0121(9) Uani 1 2 d S
F3 F 0.0000 0.5000 0.5000 0.0130(12) Uani 1 4 d S
N1 N 0.1415(7) 0.1557(5) 0.8626(5) 0.0094(8) Uani 1 1 d .
N2 N 0.4157(7) 0.2550(5) 0.7767(6) 0.0129(9) Uani 1 1 d .
N3 N 0.3480(7) 0.1557(5) 0.8610(5) 0.0107(9) Uani 1 1 d .
N4 N 0.2530(7) 0.3241(4) 0.7171(5) 0.0106(8) Uani 1 1 d .
C1 C 0.0856(8) 0.2612(6) 0.7728(7) 0.0116(10) Uani 1 1 d .
N5 N -0.1095(8) 0.2952(6) 0.7376(7) 0.0299(15) Uani 1 1 d .
H5A H -0.2083 0.2472 0.7740 0.036 Uiso 1 1 calc R
H5B H -0.1347 0.3647 0.6788 0.036 Uiso 1 1 calc R
C2 C 0.5000(8) 0.0000(6) 1.5000(7) 0.071(8) Uani 1 4 d SR
C3 C 0.1570(8) 0.0000(6) 1.5067(7) 0.032(4) Uani 0.50 2 d SPR
N6 N 0.3518(8) 0.0506(6) 1.4373(7) 0.024(5) Uani 0.25 1 d PR
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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
F2 Zn1 N4 122.26(13) . 4_565
F2 Zn1 N4 122.26(13) . .
N4 Zn1 N4 115.4(3) 4_565 .
F2 Zn1 F2 77.1(2) . 3_666
N4 Zn1 F2 95.96(15) 4_565 3_666
N4 Zn1 F2 95.96(15) . 3_666
F2 Zn1 F3 84.45(14) . .
N4 Zn1 F3 93.86(14) 4_565 .
N4 Zn1 F3 93.86(14) . .
F2 Zn1 F3 161.55(14) 3_666 .
F2 Zn1 Zn1 40.13(14) . 3_666
N4 Zn1 Zn1 113.45(14) 4_565 3_666
N4 Zn1 Zn1 113.45(13) . 3_666
F2 Zn1 Zn1 36.97(13) 3_666 3_666
F3 Zn1 Zn1 124.58(5) . 3_666
F1 Zn2 F1 180.0 3_557 .
F1 Zn2 N1 92.09(15) 3_557 4
F1 Zn2 N1 87.91(15) . 4
F1 Zn2 N1 87.91(15) 3_557 2_557
F1 Zn2 N1 92.09(15) . 2_557
N1 Zn2 N1 180.000(1) 4 2_557
F1 Zn2 N1 87.91(15) 3_557 3_557
F1 Zn2 N1 92.09(15) . 3_557
N1 Zn2 N1 90.0(2) 4 3_557
N1 Zn2 N1 90.0(2) 2_557 3_557
F1 Zn2 N1 92.09(15) 3_557 .
F1 Zn2 N1 87.91(15) . .
N1 Zn2 N1 90.0(2) 4 .
N1 Zn2 N1 90.0(2) 2_557 .
N1 Zn2 N1 179.999(1) 3_557 .
F1 Zn3 F1 180.0 . 3_657
F1 Zn3 N3 88.12(15) . 4
F1 Zn3 N3 91.88(15) 3_657 4
F1 Zn3 N3 91.88(15) . 2_657
F1 Zn3 N3 88.12(15) 3_657 2_657
N3 Zn3 N3 180.000(1) 4 2_657
F1 Zn3 N3 91.88(15) . 3_657
F1 Zn3 N3 88.12(15) 3_657 3_657
N3 Zn3 N3 91.5(2) 4 3_657
N3 Zn3 N3 88.5(2) 2_657 3_657
F1 Zn3 N3 88.12(15) . .
F1 Zn3 N3 91.88(15) 3_657 .
N3 Zn3 N3 88.5(2) 4 .
N3 Zn3 N3 91.5(2) 2_657 .
N3 Zn3 N3 179.999(1) 3_657 .
Zn3 F1 Zn2 107.8(2) . .
Zn1 F2 Zn1 102.9(2) . 3_666
Zn1 F3 Zn1 180.0 . 3_566
C1 N1 N3 105.3(4) . .
C1 N1 Zn2 138.3(4) . .
N3 N1 Zn2 116.4(3) . .
N3 N2 N4 108.1(4) . .
N2 N3 N1 110.8(4) . .
N2 N3 Zn3 132.5(4) . .
N1 N3 Zn3 116.7(3) . .
C1 N4 N2 106.3(4) . .
C1 N4 Zn1 133.4(4) . .
N2 N4 Zn1 119.8(3) . .
N1 C1 N4 109.6(5) . .
N1 C1 N5 124.9(5) . .
N4 C1 N5 125.5(5) . .
C1 N5 H5A 120.0 . .
C1 N5 H5B 120.0 . .
H5A N5 H5B 120.0 . .
C2 N6 C3 111.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 F2 1.949(5) .
Zn1 N4 2.021(4) 4_565
Zn1 N4 2.021(4) .
Zn1 F2 2.089(5) 3_666
Zn1 F3 2.1131(9) .
Zn1 Zn1 3.1596(17) 3_666
Zn2 F1 2.060(5) 3_557
Zn2 F1 2.060(5) .
Zn2 N1 2.141(4) 4
Zn2 N1 2.141(4) 2_557
Zn2 N1 2.141(4) 3_557
Zn2 N1 2.141(4) .
Zn3 F1 1.997(5) .
Zn3 F1 1.997(5) 3_657
Zn3 N3 2.168(5) 4
Zn3 N3 2.168(5) 2_657
Zn3 N3 2.168(5) 3_657
Zn3 N3 2.168(5) .
F2 Zn1 2.089(5) 3_666
F3 Zn1 2.1132(9) 3_566
N1 C1 1.334(7) .
N1 N3 1.354(6) .
N2 N3 1.290(6) .
N2 N4 1.357(6) .
N4 C1 1.349(7) .
C1 N5 1.353(7) .
N5 H5A 0.8600 .
N5 H5B 0.8600 .
C2 N6 1.2115 .
C2 N6 1.212(5) 4
C2 N6 1.212(10) 2_658
C2 N6 1.212(10) 3_658
C3 N6 1.499(4) 4
C3 N6 1.4994 .
N6 N6 0.983(12) 4
