#------------------------------------------------------------------------------
#$Date: 2021-01-07 08:23:18 +0200 (Thu, 07 Jan 2021) $
#$Revision: 260763 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/57/7705796.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_7705796
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            'C6 H16 F7 N9 O5 Ti Zn3'
_chemical_formula_weight         671.29
_space_group_IT_number           8
_space_group_name_Hall           'C -2y'
_space_group_name_H-M_alt        'C 1 m 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 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
;
2020-09-09 deposited with the CCDC.	2020-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 115.7580(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.2025(2)
_cell_length_b                   10.8541(2)
_cell_length_c                   8.8565(2)
_cell_measurement_reflns_used    2201
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      33.4
_cell_measurement_theta_min      2.23
_cell_volume                     969.89(3)
_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  0.0427
_diffrn_reflns_av_sigmaI/netI    0.0210
_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       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            33888
_diffrn_reflns_theta_full        32.61
_diffrn_reflns_theta_max         32.61
_diffrn_reflns_theta_min         2.55
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.169
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.468
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SHELX76; Sheldrick, 2008)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    2.299
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelets
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.446
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.094
_refine_diff_density_max         0.727
_refine_diff_density_min         -0.922
_refine_diff_density_rms         0.245
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.629(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         3699
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0295
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0681P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0843
_refine_ls_wR_factor_ref         0.0849
_reflns_number_gt                3661
_reflns_number_total             3699
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0dt03391j2.cif
_cod_data_source_block           trans_Zn3TiF7(H2O)2(taz)3_3H2O
_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      Cm
_cod_database_code               7705796
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.55313(6) 0.0000 0.50946(8) 0.00801(8) Uani 1 2 d S . .
Zn2 Zn 0.06600(6) 0.33878(2) 0.17190(8) 0.00783(7) Uani 1 1 d . . .
Ti1 Ti 0.0000 0.0000 0.0000 0.00885(10) Uani 1 2 d S . .
OW1 O 0.70439(19) 0.13657(18) 0.6061(3) 0.0141(3) Uani 1 1 d D . .
HW1A H 0.784(2) 0.107(4) 0.679(5) 0.063(9) Uiso 1 1 d D . .
HW1B H 0.727(4) 0.188(6) 0.543(7) 0.063(9) Uiso 1 1 d D . .
F1 F 0.1112(2) 0.5000 0.3078(3) 0.0110(3) Uani 1 2 d S . .
F2 F -0.00490(19) 0.17288(14) -0.0042(2) 0.0149(3) Uani 1 1 d . . .
F3 F -0.0717(2) 0.0000 -0.2371(3) 0.0153(4) Uani 1 2 d S . .
F4 F 0.1670(2) 0.0000 0.0035(3) 0.0175(4) Uani 1 2 d S . .
F5 F 0.0659(3) 0.0000 0.2300(3) 0.0200(4) Uani 1 2 d S . .
F6 F -0.1725(2) 0.0000 -0.0249(3) 0.0156(4) Uani 1 2 d S . .
N1 N 0.0264(2) 0.43672(17) -0.0366(2) 0.0094(3) Uani 1 1 d . . .
N2 N 0.5092(3) 0.0000 0.7168(4) 0.0112(5) Uani 1 2 d S . .
N3 N 0.42698(19) 0.20061(18) 0.2451(3) 0.0099(3) Uani 1 1 d . . .
N4 N 0.4193(2) 0.1415(2) 0.3782(3) 0.0101(3) Uani 1 1 d . . .
N5 N 0.24349(19) 0.26242(18) 0.2564(3) 0.0100(3) Uani 1 1 d . . .
C1 C 0.0157(2) 0.4027(2) -0.1853(3) 0.0110(3) Uani 1 1 d . . .
H1 H 0.0129 0.3211 -0.2186 0.013 Uiso 1 1 calc R . .
C2 C 0.3085(2) 0.1806(2) 0.3799(3) 0.0107(3) Uani 1 1 d . . .
H2 H 0.2784 0.1546 0.4574 0.013 Uiso 1 1 calc R . .
C3 C 0.3208(2) 0.2711(2) 0.1753(3) 0.0106(4) Uani 1 1 d . . .
H3 H 0.3018 0.3205 0.0819 0.013 Uiso 1 1 calc R . .
OW2 O 0.9689(5) 0.0000 0.4632(5) 0.0367(9) Uani 1 2 d SD . .
HW2A H 0.970(3) 0.0000 0.362(2) 0.063(9) Uiso 1 2 d SD . .
HW2B H 0.8814(9) 0.0000 0.435(4) 0.063(9) Uiso 1 2 d SD . .
OW3 O 0.1493(4) 0.1537(2) -0.2764(5) 0.0369(7) Uani 1 1 d D . .
HW3A H 0.212(3) 0.099(3) -0.215(7) 0.063(9) Uiso 1 1 d D . .
HW3B H 0.083(4) 0.105(3) -0.344(6) 0.063(9) Uiso 1 1 d D . .
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 95.82(8) . 2 ?
N2 Zn1 N4 95.82(8) . . ?
N4 Zn1 N4 93.55(12) 2 . ?
N2 Zn1 OW1 95.55(8) . . ?
N4 Zn1 OW1 168.31(8) 2 . ?
N4 Zn1 OW1 88.02(8) . . ?
N2 Zn1 OW1 95.55(8) . 2 ?
N4 Zn1 OW1 88.02(8) 2 2 ?
N4 Zn1 OW1 168.31(8) . 2 ?
OW1 Zn1 OW1 88.16(10) . 2 ?
N2 Zn1 F1 176.39(11) . 3_545 ?
N4 Zn1 F1 86.65(7) 2 3_545 ?
N4 Zn1 F1 86.65(7) . 3_545 ?
OW1 Zn1 F1 81.88(7) . 3_545 ?
OW1 Zn1 F1 81.88(7) 2 3_545 ?
N3 Zn2 N5 126.26(8) 4_455 . ?
N3 Zn2 N1 121.73(8) 4_455 . ?
N5 Zn2 N1 110.77(8) . . ?
N3 Zn2 F1 91.20(8) 4_455 . ?
N5 Zn2 F1 100.57(8) . . ?
N1 Zn2 F1 89.28(7) . . ?
N3 Zn2 F2 87.92(7) 4_455 . ?
N5 Zn2 F2 85.54(7) . . ?
N1 Zn2 F2 85.25(7) . . ?
F1 Zn2 F2 172.96(7) . . ?
F5 Ti1 F6 91.58(11) . . ?
F5 Ti1 F4 93.75(12) . . ?
F6 Ti1 F4 174.67(11) . . ?
F5 Ti1 F2 90.92(6) . 2 ?
F6 Ti1 F2 88.71(6) . 2 ?
F4 Ti1 F2 91.20(6) . 2 ?
F5 Ti1 F2 90.92(6) . . ?
F6 Ti1 F2 88.71(6) . . ?
F4 Ti1 F2 91.20(6) . . ?
F2 Ti1 F2 176.88(12) 2 . ?
F5 Ti1 F3 178.71(12) . . ?
F6 Ti1 F3 87.14(11) . . ?
F4 Ti1 F3 87.54(11) . . ?
F2 Ti1 F3 89.05(6) 2 . ?
F2 Ti1 F3 89.05(6) . . ?
Zn1 OW1 HW1A 114(3) . . ?
Zn1 OW1 HW1B 125(4) . . ?
HW1A OW1 HW1B 102.11(15) . . ?
Zn2 F1 Zn2 116.44(10) . 2_565 ?
Zn2 F1 Zn1 113.53(6) . 3_455 ?
Zn2 F1 Zn1 113.53(6) 2_565 3_455 ?
Ti1 F2 Zn2 140.82(9) . . ?
C1 N1 N1 106.20(13) . 2_565 ?
C1 N1 Zn2 131.08(16) . . ?
N1 N1 Zn2 122.00(5) 2_565 . ?
C1 N2 C1 103.1(3) 4_556 3_546 ?
C1 N2 Zn1 126.55(15) 4_556 . ?
C1 N2 Zn1 126.55(15) 3_546 . ?
C3 N3 N4 106.95(17) . . ?
C3 N3 Zn2 130.53(15) . 4 ?
N4 N3 Zn2 122.12(15) . 4 ?
C2 N4 N3 105.68(18) . . ?
C2 N4 Zn1 132.50(16) . . ?
N3 N4 Zn1 121.13(14) . . ?
C3 N5 C2 103.45(18) . . ?
C3 N5 Zn2 122.87(15) . . ?
C2 N5 Zn2 133.00(15) . . ?
N1 C1 N2 112.2(2) . 3_454 ?
N1 C1 H1 123.9 . . ?
N2 C1 H1 123.9 3_454 . ?
N4 C2 N5 112.38(19) . . ?
N4 C2 H2 123.8 . . ?
N5 C2 H2 123.8 . . ?
N3 C3 N5 111.54(19) . . ?
N3 C3 H3 124.2 . . ?
N5 C3 H3 124.2 . . ?
HW2A OW2 HW2B 102.12(15) . . ?
HW3A OW3 HW3B 102.11(15) . . ?
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 2.097(3) . ?
Zn1 N4 2.108(2) 2 ?
Zn1 N4 2.108(2) . ?
Zn1 OW1 2.1309(19) . ?
Zn1 OW1 2.1309(19) 2 ?
Zn1 F1 2.150(2) 3_545 ?
Zn2 N3 1.9762(18) 4_455 ?
Zn2 N5 1.9767(18) . ?
Zn2 N1 2.0060(18) . ?
Zn2 F1 2.0586(11) . ?
Zn2 F2 2.2866(16) . ?
Ti1 F5 1.841(2) . ?
Ti1 F6 1.848(2) . ?
Ti1 F4 1.858(2) . ?
Ti1 F2 1.8772(15) 2 ?
Ti1 F2 1.8772(15) . ?
Ti1 F3 1.894(2) . ?
OW1 HW1A 0.9000(10) . ?
OW1 HW1B 0.9000(10) . ?
F1 Zn2 2.0586(11) 2_565 ?
F1 Zn1 2.150(2) 3_455 ?
N1 C1 1.322(3) . ?
N1 N1 1.374(4) 2_565 ?
N2 C1 1.348(3) 4_556 ?
N2 C1 1.348(3) 3_546 ?
N3 C3 1.320(3) . ?
N3 N4 1.377(3) . ?
N3 Zn2 1.9762(18) 4 ?
N4 C2 1.318(3) . ?
N5 C3 1.348(3) . ?
N5 C2 1.350(3) . ?
C1 N2 1.348(3) 3_454 ?
C1 H1 0.9300 . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
OW2 HW2A 0.9000(10) . ?
OW2 HW2B 0.9000(10) . ?
OW3 HW3A 0.9000(10) . ?
OW3 HW3B 0.9000(10) . ?
