#------------------------------------------------------------------------------
#$Date: 2024-03-05 04:01:54 +0200 (Tue, 05 Mar 2024) $
#$Revision: 290296 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/11/1571112.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_1571112
loop_
_publ_author_name
'Seo, Jun Min'
'Jo, Hongil'
'Choi, Myung Ho'
'Ok, Kang Min'
'Chang, Hong Young'
'Kim, Sun Woo'
_publ_section_title
;
 Polymorphisms in M2+AlF5(H2O)7 (M2+ = Fe2+, Co2+, or Ni2+): Syntheses,
 Crystal Structures, and Characterization of New Mixed Metal Fluoride
 Hydrates
;
_journal_issue                   2
_journal_name_full               Crystals
_journal_page_first              197
_journal_paper_doi               10.3390/cryst14020197
_journal_volume                  14
_journal_year                    2024
_chemical_formula_sum            'Al F5 Fe H14 O7'
_chemical_formula_weight         303.94
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_cell_angle_alpha                103.834(3)
_cell_angle_beta                 96.364(3)
_cell_angle_gamma                95.400(3)
_cell_formula_units_Z            2
_cell_length_a                   6.4864(9)
_cell_length_b                   8.7190(11)
_cell_length_c                   8.7917(11)
_cell_measurement_reflns_used    8644
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.96
_cell_volume                     476.05(11)
_computing_cell_refinement       'SAINT V8.40A integration software'
_computing_data_collection       'Bruker APEX3 software'
_computing_data_reduction        'SAINT V8.40A integration software'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9275
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         2.409
_diffrn_source                   'sealed x-ray tube'
_exptl_absorpt_coefficient_mu    1.770
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6062
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.120
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             308
_exptl_crystal_size_max          0.158
_exptl_crystal_size_mid          0.046
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.472
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         1733
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0354P)²+2.9035P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1133
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1685
_reflns_number_total             1733
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            Total_final.cif
_cod_data_source_block           FeAlF_100K
_cod_database_code               1571112
_shelx_shelxl_version_number     2019/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.767
_shelx_estimated_absorpt_t_max   0.928
loop_
_space_group_symop_operation_xyz
'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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.500000 0.500000 0.500000 0.0108(2) Uani 1 2 d S . P . .
Fe2 Fe 0.500000 0.000000 1.000000 0.0105(2) Uani 1 2 d S . P . .
Al1 Al 0.000000 0.000000 0.500000 0.0093(4) Uani 1 2 d S . P . .
Al2 Al 1.000000 0.500000 1.000000 0.0082(4) Uani 1 2 d S . P . .
O1 O -0.0391(6) 0.2182(5) 0.5276(6) 0.0310(11) Uani 0.5 1 d D . P . .
H1A H 0.032(18) 0.282(17) 0.626(10) 0.047 Uiso 0.5 1 d D U P . .
H1B H -0.180(8) 0.239(18) 0.525(16) 0.047 Uiso 0.5 1 d D U P . .
O2 O 0.8985(6) 0.5732(5) 1.1921(4) 0.0200(8) Uani 0.5 1 d D . P . .
H2A H 0.819(19) 0.507(13) 1.243(13) 0.030 Uiso 0.5 1 d D U P . .
H2B H 0.97(2) 0.658(11) 1.276(10) 0.030 Uiso 0.5 1 d D U P . .
O3 O 0.5308(8) 0.3243(5) 0.6254(5) 0.0292(12) Uani 1 1 d D . . . .
H3A H 0.454(11) 0.398(6) 0.686(9) 0.044 Uiso 1 1 d D U . . .
H3B H 0.449(10) 0.225(4) 0.619(9) 0.044 Uiso 1 1 d D U . . .
O4 O 0.2201(5) 0.3721(5) 0.3692(5) 0.0172(7) Uani 1 1 d D . . . .
H4A H 0.115(7) 0.324(8) 0.414(7) 0.026 Uiso 1 1 d D U . . .
H4B H 0.164(9) 0.381(8) 0.268(4) 0.026 Uiso 1 1 d D U . . .
O5 O 0.3122(6) 0.6270(5) 0.6596(5) 0.0210(9) Uani 1 1 d D . . . .
H5A H 0.255(11) 0.709(6) 0.623(7) 0.032 Uiso 1 1 d D U . . .
H5B H 0.392(10) 0.669(7) 0.760(4) 0.032 Uiso 1 1 d D U . . .
O6 O 0.1827(5) -0.0693(5) 0.9190(5) 0.0173(8) Uani 1 1 d D . . . .
H6A H 0.108(9) -0.021(7) 0.849(7) 0.026 Uiso 1 1 d D U . . .
H6B H 0.091(8) -0.148(6) 0.941(8) 0.026 Uiso 1 1 d D U . . .
O7 O 0.5542(6) -0.0354(5) 0.7631(5) 0.0184(9) Uani 1 1 d D . . . .
H7A H 0.462(8) 0.004(9) 0.697(7) 0.028 Uiso 1 1 d D U . . .
H7B H 0.687(5) -0.020(9) 0.732(8) 0.028 Uiso 1 1 d D U . . .
O8 O 0.4577(7) 0.2447(5) 1.0255(5) 0.0185(9) Uani 1 1 d D . . . .
H8A H 0.331(6) 0.284(8) 1.000(8) 0.028 Uiso 1 1 d D U . . .
H8B H 0.561(7) 0.308(7) 0.992(8) 0.028 Uiso 1 1 d D U . . .
F1 F -0.0391(6) 0.2182(5) 0.5276(6) 0.0310(11) Uani 0.5 1 d . . P . .
F2 F 0.8985(6) 0.5732(5) 1.1921(4) 0.0200(8) Uani 0.5 1 d . . P . .
F3 F 0.0565(6) -0.0056(6) 0.3066(4) 0.0326(10) Uani 1 1 d . . . . .
F4 F 0.2721(5) 0.0568(4) 0.5744(4) 0.0166(7) Uani 1 1 d . . . . .
F5 F 0.7450(5) 0.3992(4) 0.9127(4) 0.0169(7) Uani 1 1 d . . . . .
F6 F 0.9310(5) 0.6755(4) 0.9406(4) 0.0166(7) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 '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
_geom_angle_publ_flag
O4 Fe1 O4 180.0 2_666 . ?
O4 Fe1 O3 90.57(18) 2_666 2_666 ?
O4 Fe1 O3 89.43(18) . 2_666 ?
O4 Fe1 O3 89.43(18) 2_666 . ?
O4 Fe1 O3 90.57(19) . . ?
O3 Fe1 O3 180.0 2_666 . ?
O4 Fe1 O5 87.05(14) 2_666 2_666 ?
O4 Fe1 O5 92.95(14) . 2_666 ?
O3 Fe1 O5 93.18(19) 2_666 2_666 ?
O3 Fe1 O5 86.82(19) . 2_666 ?
O4 Fe1 O5 92.95(14) 2_666 . ?
O4 Fe1 O5 87.05(14) . . ?
O3 Fe1 O5 86.82(19) 2_666 . ?
O3 Fe1 O5 93.18(19) . . ?
O5 Fe1 O5 180.0 2_666 . ?
O6 Fe2 O6 180.0(2) 2_657 . ?
O6 Fe2 O7 91.38(17) 2_657 . ?
O6 Fe2 O7 88.62(17) . . ?
O6 Fe2 O7 88.62(17) 2_657 2_657 ?
O6 Fe2 O7 91.38(17) . 2_657 ?
O7 Fe2 O7 180.0 . 2_657 ?
O6 Fe2 O8 90.78(16) 2_657 2_657 ?
O6 Fe2 O8 89.22(17) . 2_657 ?
O7 Fe2 O8 86.26(15) . 2_657 ?
O7 Fe2 O8 93.74(15) 2_657 2_657 ?
O6 Fe2 O8 89.22(17) 2_657 . ?
O6 Fe2 O8 90.78(16) . . ?
O7 Fe2 O8 93.74(15) . . ?
O7 Fe2 O8 86.26(15) 2_657 . ?
O8 Fe2 O8 180.0(2) 2_657 . ?
F3 Al1 F3 180.0 2_556 . ?
F3 Al1 F4 90.29(16) 2_556 . ?
F3 Al1 F4 89.71(16) . . ?
F3 Al1 F4 89.71(16) 2_556 2_556 ?
F3 Al1 F4 90.29(16) . 2_556 ?
F4 Al1 F4 180.0 . 2_556 ?
F3 Al1 O1 89.1(2) 2_556 2_556 ?
F3 Al1 O1 90.9(2) . 2_556 ?
F4 Al1 O1 89.91(15) . 2_556 ?
F4 Al1 O1 90.09(15) 2_556 2_556 ?
F3 Al1 O1 90.9(2) 2_556 . ?
F3 Al1 O1 89.1(2) . . ?
F4 Al1 O1 90.09(15) . . ?
F4 Al1 O1 89.91(15) 2_556 . ?
O1 Al1 O1 180.0 2_556 . ?
F5 Al2 F5 180.0 2_767 . ?
F5 Al2 F6 89.37(16) 2_767 2_767 ?
F5 Al2 F6 90.63(16) . 2_767 ?
F5 Al2 F6 90.63(16) 2_767 . ?
F5 Al2 F6 89.37(16) . . ?
F6 Al2 F6 180.00(7) 2_767 . ?
F5 Al2 O2 90.06(16) 2_767 . ?
F5 Al2 O2 89.94(16) . . ?
F6 Al2 O2 90.32(16) 2_767 . ?
F6 Al2 O2 89.68(16) . . ?
F5 Al2 O2 89.94(16) 2_767 2_767 ?
F5 Al2 O2 90.06(16) . 2_767 ?
F6 Al2 O2 89.68(16) 2_767 2_767 ?
F6 Al2 O2 90.31(16) . 2_767 ?
O2 Al2 O2 180.0 . 2_767 ?
Al1 O1 H1A 111(10) . . ?
Al1 O1 H1B 115(10) . . ?
H1A O1 H1B 106(5) . . ?
Al2 O2 H2A 125(8) . . ?
Al2 O2 H2B 124(8) . . ?
H2A O2 H2B 105(5) . . ?
Fe1 O3 H3A 75(5) . . ?
Fe1 O3 H3B 133(5) . . ?
H3A O3 H3B 102(4) . . ?
Fe1 O4 H4A 124(4) . . ?
Fe1 O4 H4B 124(4) . . ?
H4A O4 H4B 110(4) . . ?
Fe1 O5 H5A 113(5) . . ?
Fe1 O5 H5B 110(4) . . ?
H5A O5 H5B 110(4) . . ?
Fe2 O6 H6A 122(4) . . ?
Fe2 O6 H6B 130(4) . . ?
H6A O6 H6B 108(4) . . ?
Fe2 O7 H7A 117(4) . . ?
Fe2 O7 H7B 124(4) . . ?
H7A O7 H7B 106(4) . . ?
Fe2 O8 H8A 126(4) . . ?
Fe2 O8 H8B 116(4) . . ?
H8A O8 H8B 105(4) . . ?
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
Fe1 O4 2.099(3) 2_666 ?
Fe1 O4 2.099(3) . ?
Fe1 O3 2.102(4) 2_666 ?
Fe1 O3 2.102(4) . ?
Fe1 O5 2.138(4) 2_666 ?
Fe1 O5 2.138(4) . ?
Fe2 O6 2.084(3) 2_657 ?
Fe2 O6 2.084(3) . ?
Fe2 O7 2.105(4) . ?
Fe2 O7 2.105(4) 2_657 ?
Fe2 O8 2.138(4) 2_657 ?
Fe2 O8 2.139(4) . ?
Al1 F3 1.769(4) 2_556 ?
Al1 F3 1.769(4) . ?
Al1 F4 1.793(3) . ?
Al1 F4 1.793(3) 2_556 ?
Al1 O1 1.904(4) 2_556 ?
Al1 O1 1.904(4) . ?
Al2 F5 1.794(3) 2_767 ?
Al2 F5 1.794(3) . ?
Al2 F6 1.809(3) 2_767 ?
Al2 F6 1.809(3) . ?
Al2 O2 1.872(4) . ?
Al2 O2 1.872(4) 2_767 ?
O1 H1A 0.95(2) . ?
O1 H1B 0.95(2) . ?
O2 H2A 0.95(2) . ?
O2 H2B 0.95(2) . ?
O3 H3A 0.95(2) . ?
O3 H3B 0.96(2) . ?
O4 H4A 0.94(2) . ?
O4 H4B 0.95(2) . ?
O5 H5A 0.94(2) . ?
O5 H5B 0.94(2) . ?
O6 H6A 0.94(2) . ?
O6 H6B 0.94(2) . ?
O7 H7A 0.94(2) . ?
O7 H7B 0.94(2) . ?
O8 H8A 0.94(2) . ?
O8 H8B 0.94(2) . ?
