#------------------------------------------------------------------------------
#$Date: 2021-01-07 08:23:18 +0200 (Thu, 07 Jan 2021) $
#$Revision: 260763 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/58/7705800.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_7705800
loop_
_publ_author_name
'Albino, M.'
'Lhoste, J.'
'Body, M.'
'Legein, C.'
'Hémon-Ribaud, A'
'Maisonneuve, V.'
'Leblanc, M.'
_publ_section_title
;
 Topotactic desolvation and condensation reactions of 3D
 Zn₃TiF₇(H₂O)₂(taz)₃·S
 (S = 3H₂O or C₂H₅OH).
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17758
_journal_page_last               17771
_journal_paper_doi               10.1039/d0dt03391j
_journal_volume                  49
_journal_year                    2020
_chemical_formula_sum            'C8 H16 F7 N9 O3 Ti Zn3'
_chemical_formula_weight         663.31
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2020-09-09 deposited with the CCDC.	2020-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.020(11)
_cell_length_b                   10.292(7)
_cell_length_c                   11.213(7)
_cell_measurement_reflns_used    298
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.2
_cell_measurement_theta_min      2.7
_cell_volume                     1964(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0940
_diffrn_reflns_av_sigmaI/netI    0.0518
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            25740
_diffrn_reflns_theta_full        28.23
_diffrn_reflns_theta_max         28.23
_diffrn_reflns_theta_min         2.39
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.109
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.639
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SHELX76; Sheldrick, 2008)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    2.243
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.167
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.734
_refine_diff_density_min         -0.710
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         2560
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0394
_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)+(0.0543P)²+0.7785P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1131
_reflns_number_gt                1886
_reflns_number_total             2560
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0dt03391j2.cif
_cod_data_source_block           cis_Zn3TiF7(H2O)2(taz)3_EtOH
_cod_depositor_comments
;
The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7705796--7705801.cif.
;
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               7705800
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x+1/2, -y, z+1/2'
'-x, -y, -z'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'
'x-1/2, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.12200(4) 0.2500 0.30748(6) 0.01532(18) Uani 1 2 d S . .
Zn2 Zn 0.29956(3) 0.42079(5) 0.37716(4) 0.01670(15) Uani 1 1 d . . .
Ti1 Ti 0.44253(6) 0.7500 0.29718(10) 0.0182(3) Uani 1 2 d S . .
F1 F 0.23546(19) 0.2500 0.3991(3) 0.0190(8) Uani 1 2 d S . .
F2 F 0.37119(14) 0.6145(3) 0.3351(2) 0.0290(6) Uani 1 1 d . . .
F3 F 0.3966(3) 0.7500 0.1443(3) 0.0388(11) Uani 1 2 d S . .
F4 F 0.51452(18) 0.8719(3) 0.2470(3) 0.0472(9) Uani 1 1 d . . .
F5 F 0.4775(3) 0.7500 0.4486(4) 0.0547(14) Uani 1 2 d S . .
OW1 O 0.0856(3) 0.3923(7) 0.4327(5) 0.0794(19) Uani 1 1 d D . .
H1WA H 0.061(6) 0.470(5) 0.430(9) 0.17(4) Uiso 1 1 d D . .
H1WB H 0.065(6) 0.357(9) 0.499(6) 0.17(4) Uiso 1 1 d D . .
N1 N -0.10436(19) 0.3177(3) 0.1635(3) 0.0182(8) Uani 1 1 d . . .
C1 C -0.0341(2) 0.3515(4) 0.1987(4) 0.0205(10) Uani 1 1 d . . .
H1 H -0.0181 0.4375 0.2064 0.025 Uiso 1 1 calc R . .
N2 N 0.0126(3) 0.2500 0.2227(5) 0.0182(11) Uani 1 2 d S . .
N3 N 0.23854(19) 0.4676(3) 0.2303(3) 0.0166(7) Uani 1 1 d . . .
N4 N 0.1710(2) 0.3990(4) 0.2020(3) 0.0183(8) Uani 1 1 d . . .
C2 C 0.1533(3) 0.4305(5) 0.0923(4) 0.0208(10) Uani 1 1 d . . .
H2 H 0.1100 0.3977 0.0516 0.025 Uiso 1 1 calc R . .
C3 C 0.2561(3) 0.5356(4) 0.1340(4) 0.0198(9) Uani 1 1 d . . .
H3 H 0.2991 0.5910 0.1286 0.024 Uiso 1 1 calc R . .
N5 N 0.29531(19) 0.4844(4) 0.5444(3) 0.0181(8) Uani 1 1 d . . .
C1E C 0.6755(6) 0.7500 0.0852(11) 0.068(3) Uani 1 2 d S . .
C2E C 0.6144(7) 0.7692(14) -0.0098(12) 0.081(6) Uani 0.50 1 d PD . .
O1E O 0.5623(4) 0.8764(8) 0.0343(7) 0.044(2) Uani 0.50 1 d PD . .
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'
Ti Ti 0.2776 0.4457 '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
_geom_angle_publ_flag
N2 Zn1 N4 95.59(14) . . ?
N2 Zn1 N4 95.59(14) . 7_565 ?
N4 Zn1 N4 93.3(2) . 7_565 ?
N2 Zn1 OW1 92.34(17) . 7_565 ?
N4 Zn1 OW1 171.44(18) . 7_565 ?
N4 Zn1 OW1 89.1(2) 7_565 7_565 ?
N2 Zn1 OW1 92.34(17) . . ?
N4 Zn1 OW1 89.1(2) . . ?
N4 Zn1 OW1 171.45(18) 7_565 . ?
OW1 Zn1 OW1 87.3(4) 7_565 . ?
N2 Zn1 F1 179.05(17) . . ?
N4 Zn1 F1 85.06(12) . . ?
N4 Zn1 F1 85.06(12) 7_565 . ?
OW1 Zn1 F1 86.98(15) 7_565 . ?
OW1 Zn1 F1 86.98(15) . . ?
N5 Zn2 N1 114.77(15) . 8_656 ?
N5 Zn2 N3 132.60(15) . . ?
N1 Zn2 N3 111.31(15) 8_656 . ?
N5 Zn2 F1 98.47(14) . . ?
N1 Zn2 F1 90.43(13) 8_656 . ?
N3 Zn2 F1 91.61(14) . . ?
N5 Zn2 F2 85.98(13) . . ?
N1 Zn2 F2 88.89(12) 8_656 . ?
N3 Zn2 F2 84.36(12) . . ?
F1 Zn2 F2 175.36(12) . . ?
F5 Ti1 F4 93.90(16) . 7_575 ?
F5 Ti1 F4 93.90(16) . . ?
F4 Ti1 F4 85.89(19) 7_575 . ?
F5 Ti1 F3 174.8(2) . . ?
F4 Ti1 F3 89.89(17) 7_575 . ?
F4 Ti1 F3 89.89(17) . . ?
F5 Ti1 F2 90.00(14) . 7_575 ?
F4 Ti1 F2 174.25(14) 7_575 7_575 ?
F4 Ti1 F2 89.64(13) . 7_575 ?
F3 Ti1 F2 86.50(13) . 7_575 ?
F5 Ti1 F2 90.00(14) . . ?
F4 Ti1 F2 89.64(13) 7_575 . ?
F4 Ti1 F2 174.25(14) . . ?
F3 Ti1 F2 86.50(13) . . ?
F2 Ti1 F2 94.59(18) 7_575 . ?
Zn2 F1 Zn2 115.06(16) 7_565 . ?
Zn2 F1 Zn1 114.02(10) 7_565 . ?
Zn2 F1 Zn1 114.02(10) . . ?
Ti1 F2 Zn2 170.48(15) . . ?
Zn1 OW1 H1WA 136(7) . . ?
Zn1 OW1 H1WB 112(7) . . ?
H1WA OW1 H1WB 102.2(10) . . ?
C1 N1 N1 105.5(2) . 7_565 ?
C1 N1 Zn2 132.5(3) . 8_556 ?
N1 N1 Zn2 122.01(10) 7_565 8_556 ?
N1 C1 N2 113.3(4) . . ?
N1 C1 H1 123.3 . . ?
N2 C1 H1 123.3 . . ?
C1 N2 C1 102.5(5) 7_565 . ?
C1 N2 Zn1 128.3(2) 7_565 . ?
C1 N2 Zn1 128.3(2) . . ?
C3 N3 N4 105.7(3) . . ?
C3 N3 Zn2 132.9(3) . . ?
N4 N3 Zn2 119.7(3) . . ?
C2 N4 N3 106.3(3) . . ?
C2 N4 Zn1 128.1(3) . . ?
N3 N4 Zn1 124.8(3) . . ?
N4 C2 N5 112.7(4) . 4_564 ?
N4 C2 H2 123.7 . . ?
N5 C2 H2 123.7 4_564 . ?
N3 C3 N5 112.4(4) . 4_564 ?
N3 C3 H3 123.8 . . ?
N5 C3 H3 123.8 4_564 . ?
C3 N5 C2 102.9(3) 4_565 4_565 ?
C3 N5 Zn2 132.6(3) 4_565 . ?
C2 N5 Zn2 124.4(3) 4_565 . ?
C2E C1E C2E 15.1(11) 7_575 . ?
C2E C2E O1E 137.4(7) 7_575 . ?
C2E C2E C1E 82.4(5) 7_575 . ?
O1E C2E C1E 105.8(8) . . ?
C2E C2E O1E 34.1(3) 7_575 7_575 ?
O1E C2E O1E 103.2(9) . 7_575 ?
C1E C2E O1E 92.1(9) . 7_575 ?
C2E O1E C2E 8.5(6) . 7_575 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 N2 2.090(5) . ?
Zn1 N4 2.109(4) . ?
Zn1 N4 2.109(4) 7_565 ?
Zn1 OW1 2.121(5) 7_565 ?
Zn1 OW1 2.121(5) . ?
Zn1 F1 2.187(4) . ?
Zn2 N5 1.988(4) . ?
Zn2 N1 2.002(3) 8_656 ?
Zn2 N3 2.006(4) . ?
Zn2 F1 2.083(2) . ?
Zn2 F2 2.384(3) . ?
Ti1 F5 1.799(4) . ?
Ti1 F4 1.841(3) 7_575 ?
Ti1 F4 1.842(3) . ?
Ti1 F3 1.884(4) . ?
Ti1 F2 1.897(3) 7_575 ?
Ti1 F2 1.897(3) . ?
F1 Zn2 2.083(2) 7_565 ?
OW1 H1WA 0.9000(12) . ?
OW1 H1WB 0.9000(11) . ?
N1 C1 1.307(5) . ?
N1 N1 1.393(7) 7_565 ?
N1 Zn2 2.002(3) 8_556 ?
C1 N2 1.340(5) . ?
C1 H1 0.9300 . ?
N2 C1 1.340(5) 7_565 ?
N3 C3 1.321(5) . ?
N3 N4 1.385(5) . ?
N4 C2 1.307(5) . ?
C2 N5 1.349(5) 4_564 ?
C2 H2 0.9300 . ?
C3 N5 1.348(5) 4_564 ?
C3 H3 0.9300 . ?
N5 C3 1.348(5) 4_565 ?
N5 C2 1.349(5) 4_565 ?
C1E C2E 1.501(16) 7_575 ?
C1E C2E 1.501(16) . ?
C2E C2E 0.40(3) 7_575 ?
C2E O1E 1.5000(12) . ?
C2E O1E 1.81(2) 7_575 ?
O1E C2E 1.81(2) 7_575 ?
