#------------------------------------------------------------------------------
#$Date: 2024-03-05 04:01:54 +0200 (Tue, 05 Mar 2024) $
#$Revision: 290296 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/11/1571114.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_1571114
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 H14 Ni O7'
_chemical_formula_weight         306.80
_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                104.255(3)
_cell_angle_beta                 96.638(3)
_cell_angle_gamma                94.816(3)
_cell_formula_units_Z            2
_cell_length_a                   6.4022(6)
_cell_length_b                   8.5874(7)
_cell_length_c                   8.7691(7)
_cell_measurement_reflns_used    8180
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      2.97
_cell_volume                     460.96(7)
_computing_cell_refinement       'SAINT V8.40A integration software'
_computing_data_collection       'Bruker APEX3 software'
_computing_data_reduction        'Bruker APEX3 software'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      101(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0435
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_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            13295
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.346
_diffrn_reflns_theta_min         2.421
_diffrn_source                   'sealed x-ray tube'
_exptl_absorpt_coefficient_mu    2.296
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6076
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.210
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             312
_exptl_crystal_size_max          0.158
_exptl_crystal_size_mid          0.046
_exptl_crystal_size_min          0.043
_refine_diff_density_max         2.001
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         1688
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0512
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0574P)²+4.5672P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1377
_refine_ls_wR_factor_ref         0.1408
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1576
_reflns_number_total             1688
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            Total_final.cif
_cod_data_source_block           NIAlF_100K
_cod_database_code               1571114
_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   0.713
_shelx_estimated_absorpt_t_max   0.908
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
Ni1 Ni 0.500000 0.500000 0.500000 0.0078(3) Uani 1 2 d S . P . .
Ni2 Ni 0.500000 0.000000 1.000000 0.0074(3) Uani 1 2 d S . P . .
Al1 Al 0.000000 0.000000 0.500000 0.0096(5) Uani 1 2 d S . P . .
Al2 Al 1.000000 0.500000 1.000000 0.0090(5) Uani 1 2 d S . P . .
O1 O -0.0374(6) 0.2204(5) 0.5313(6) 0.0272(11) Uani 0.5 1 d D . P . .
H1A H -0.138(18) 0.20(2) 0.596(17) 0.041 Uiso 0.5 1 d D U P . .
H1B H -0.10(2) 0.282(19) 0.466(16) 0.041 Uiso 0.5 1 d D U P . .
O2 O 0.8861(6) 0.5748(5) 1.1875(5) 0.0162(8) Uani 0.5 1 d D . P . .
H2A H 0.88(2) 0.487(9) 1.236(13) 0.024 Uiso 0.5 1 d D U P . .
H2B H 0.93(2) 0.666(9) 1.276(9) 0.024 Uiso 0.5 1 d D U P . .
O3 O 0.5355(7) 0.3246(5) 0.6178(5) 0.0205(10) Uani 1 1 d D . . . .
H3A H 0.456(10) 0.386(7) 0.691(8) 0.031 Uiso 1 1 d D U . . .
H3B H 0.453(10) 0.221(4) 0.590(9) 0.031 Uiso 1 1 d D U . . .
O4 O 0.2212(6) 0.3793(5) 0.3734(5) 0.0135(9) Uani 1 1 d D . . . .
H4A H 0.119(9) 0.322(7) 0.416(7) 0.020 Uiso 1 1 d D U . . .
H4B H 0.191(10) 0.338(8) 0.262(2) 0.020 Uiso 1 1 d D U . . .
O5 O 0.3220(6) 0.6250(5) 0.6603(5) 0.0175(9) Uani 1 1 d D . . . .
H5A H 0.224(9) 0.697(7) 0.641(8) 0.026 Uiso 1 1 d D U . . .
H5B H 0.418(9) 0.687(7) 0.748(6) 0.026 Uiso 1 1 d D U . . .
O6 O 0.1886(6) -0.0665(5) 0.9246(5) 0.0150(9) Uani 1 1 d D . . . .
H6A H 0.116(9) -0.013(7) 0.857(7) 0.023 Uiso 1 1 d D U . . .
H6B H 0.097(9) -0.150(6) 0.942(8) 0.023 Uiso 1 1 d D U . . .
O7 O 0.5540(6) -0.0391(5) 0.7678(5) 0.0135(9) Uani 1 1 d D . . . .
H7A H 0.458(8) -0.004(9) 0.698(6) 0.020 Uiso 1 1 d D U . . .
H7B H 0.677(7) -0.062(9) 0.722(7) 0.020 Uiso 1 1 d D U . . .
O8 O 0.4580(7) 0.2388(5) 1.0191(5) 0.0147(9) Uani 1 1 d D . . . .
H8A H 0.330(6) 0.283(8) 1.029(9) 0.022 Uiso 1 1 d D U . . .
H8B H 0.549(8) 0.301(7) 0.975(8) 0.022 Uiso 1 1 d D U . . .
F1 F -0.0374(6) 0.2204(5) 0.5313(6) 0.0272(11) Uani 0.5 1 d . . P . .
F2 F 0.8861(6) 0.5748(5) 1.1875(5) 0.0162(8) Uani 0.5 1 d . . P . .
F3 F 0.0554(6) -0.0041(6) 0.3034(4) 0.0262(9) Uani 1 1 d . . . . .
F4 F 0.2755(5) 0.0568(4) 0.5732(4) 0.0139(7) Uani 1 1 d . . . . .
F5 F 0.7461(5) 0.3959(4) 0.9065(4) 0.0133(7) Uani 1 1 d . . . . .
F6 F 0.9318(5) 0.6765(4) 0.9379(4) 0.0133(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'
Ni Ni 0.3393 1.1124 '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 Ni1 O4 180.0 . 2_666 ?
O4 Ni1 O3 91.41(17) . . ?
O4 Ni1 O3 88.59(17) 2_666 . ?
O4 Ni1 O3 88.59(17) . 2_666 ?
O4 Ni1 O3 91.41(17) 2_666 2_666 ?
O3 Ni1 O3 180.0 . 2_666 ?
O4 Ni1 O5 92.97(16) . 2_666 ?
O4 Ni1 O5 87.03(16) 2_666 2_666 ?
O3 Ni1 O5 86.72(19) . 2_666 ?
O3 Ni1 O5 93.28(19) 2_666 2_666 ?
O4 Ni1 O5 87.03(16) . . ?
O4 Ni1 O5 92.97(16) 2_666 . ?
O3 Ni1 O5 93.28(19) . . ?
O3 Ni1 O5 86.72(19) 2_666 . ?
O5 Ni1 O5 180.0 2_666 . ?
O6 Ni2 O6 180.0 . 2_657 ?
O6 Ni2 O7 89.66(17) . . ?
O6 Ni2 O7 90.34(17) 2_657 . ?
O6 Ni2 O7 90.34(17) . 2_657 ?
O6 Ni2 O7 89.66(17) 2_657 2_657 ?
O7 Ni2 O7 180.0 . 2_657 ?
O6 Ni2 O8 89.45(17) . 2_657 ?
O6 Ni2 O8 90.55(17) 2_657 2_657 ?
O7 Ni2 O8 87.04(17) . 2_657 ?
O7 Ni2 O8 92.96(17) 2_657 2_657 ?
O6 Ni2 O8 90.55(17) . . ?
O6 Ni2 O8 89.45(17) 2_657 . ?
O7 Ni2 O8 92.96(17) . . ?
O7 Ni2 O8 87.04(17) 2_657 . ?
O8 Ni2 O8 180.0 2_657 . ?
F4 Al1 F4 180.0 2_556 . ?
F4 Al1 F3 89.46(16) 2_556 2_556 ?
F4 Al1 F3 90.54(16) . 2_556 ?
F4 Al1 F3 90.54(16) 2_556 . ?
F4 Al1 F3 89.46(16) . . ?
F3 Al1 F3 180.0 2_556 . ?
F4 Al1 O1 89.38(16) 2_556 2_556 ?
F4 Al1 O1 90.62(16) . 2_556 ?
F3 Al1 O1 88.9(2) 2_556 2_556 ?
F3 Al1 O1 91.1(2) . 2_556 ?
F4 Al1 O1 90.62(16) 2_556 . ?
F4 Al1 O1 89.38(16) . . ?
F3 Al1 O1 91.1(2) 2_556 . ?
F3 Al1 O1 88.9(2) . . ?
O1 Al1 O1 180.0 2_556 . ?
F4 Al1 H1A 76(4) 2_556 . ?
F4 Al1 H1A 104(4) . . ?
F3 Al1 H1A 68(3) 2_556 . ?
F3 Al1 H1A 112(3) . . ?
O1 Al1 H1A 151.9(18) 2_556 . ?
O1 Al1 H1A 28.1(17) . . ?
F5 Al2 F5 180.0 2_767 . ?
F5 Al2 F6 89.69(15) 2_767 2_767 ?
F5 Al2 F6 90.31(15) . 2_767 ?
F5 Al2 F6 90.31(15) 2_767 . ?
F5 Al2 F6 89.69(15) . . ?
F6 Al2 F6 180.00(8) 2_767 . ?
F5 Al2 O2 89.53(16) 2_767 2_767 ?
F5 Al2 O2 90.47(16) . 2_767 ?
F6 Al2 O2 89.62(16) 2_767 2_767 ?
F6 Al2 O2 90.38(16) . 2_767 ?
F5 Al2 O2 90.47(16) 2_767 . ?
F5 Al2 O2 89.53(16) . . ?
F6 Al2 O2 90.38(16) 2_767 . ?
F6 Al2 O2 89.62(16) . . ?
O2 Al2 O2 180.0(3) 2_767 . ?
Al1 O1 H1A 83(10) . . ?
Al1 O1 H1B 134(10) . . ?
H1A O1 H1B 107(5) . . ?
Al2 O2 H2A 105(8) . . ?
Al2 O2 H2B 130(9) . . ?
H2A O2 H2B 103(4) . . ?
Ni1 O3 H3A 85(5) . . ?
Ni1 O3 H3B 125(5) . . ?
H3A O3 H3B 101(4) . . ?
Ni1 O4 H4A 124(4) . . ?
Ni1 O4 H4B 127(4) . . ?
H4A O4 H4B 106(4) . . ?
Ni1 O5 H5A 127(5) . . ?
Ni1 O5 H5B 107(4) . . ?
H5A O5 H5B 104(4) . . ?
Ni2 O6 H6A 119(4) . . ?
Ni2 O6 H6B 130(4) . . ?
H6A O6 H6B 110(4) . . ?
Ni2 O7 H7A 117(4) . . ?
Ni2 O7 H7B 131(4) . . ?
H7A O7 H7B 110(4) . . ?
Ni2 O8 H8A 126(4) . . ?
Ni2 O8 H8B 119(4) . . ?
H8A O8 H8B 110(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
Ni1 O4 2.039(4) . ?
Ni1 O4 2.039(4) 2_666 ?
Ni1 O3 2.039(4) . ?
Ni1 O3 2.039(4) 2_666 ?
Ni1 O5 2.064(4) 2_666 ?
Ni1 O5 2.064(4) . ?
Ni2 O6 2.014(4) . ?
Ni2 O6 2.014(4) 2_657 ?
Ni2 O7 2.055(4) . ?
Ni2 O7 2.055(4) 2_657 ?
Ni2 O8 2.058(4) 2_657 ?
Ni2 O8 2.058(4) . ?
Al1 F4 1.789(3) 2_556 ?
Al1 F4 1.789(3) . ?
Al1 F3 1.793(4) 2_556 ?
Al1 F3 1.793(4) . ?
Al1 O1 1.884(4) 2_556 ?
Al1 O1 1.884(4) . ?
Al1 H1A 2.01(15) . ?
Al2 F5 1.789(3) 2_767 ?
Al2 F5 1.789(3) . ?
Al2 F6 1.802(3) 2_767 ?
Al2 F6 1.802(3) . ?
Al2 O2 1.867(4) 2_767 ?
Al2 O2 1.867(4) . ?
O1 H1A 0.95(2) . ?
O1 H1B 0.95(2) . ?
O2 H2A 0.95(2) . ?
O2 H2B 0.96(2) . ?
O3 H3A 0.95(2) . ?
O3 H3B 0.95(2) . ?
O4 H4A 0.95(2) . ?
O4 H4B 0.94(2) . ?
O5 H5A 0.95(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) . ?
