#------------------------------------------------------------------------------
#$Date: 2024-03-05 03:01:54 +0100 (Tue 05 de Mar de 2024) $
#$Revision: 290296 $
#$URL: svn://www.crystallography.net/cod/cif/1/57/11/1571113.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_1571113
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 Co F5 H14 O7'
_chemical_formula_weight         307.02
_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                104.019(2)
_cell_angle_beta                 96.749(2)
_cell_angle_gamma                95.254(2)
_cell_formula_units_Z            2
_cell_length_a                   6.4434(5)
_cell_length_b                   8.6691(6)
_cell_length_c                   8.8031(6)
_cell_measurement_reflns_used    9864
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.41
_cell_measurement_theta_min      2.96
_cell_volume                     470.08(6)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_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            13330
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.410
_diffrn_source                   'sealed x-ray tube'
_exptl_absorpt_coefficient_mu    2.014
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6343
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.169
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             310
_exptl_crystal_size_max          0.158
_exptl_crystal_size_mid          0.046
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         1723
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0329
_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)+1.8062P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0743
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1608
_reflns_number_total             1723
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            Total_final.cif
_cod_data_source_block           CoAlF_100K
_cod_database_code               1571113
_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   0.741
_shelx_estimated_absorpt_t_max   0.918
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
Co1 Co 0.500000 0.500000 0.500000 0.00844(17) Uani 1 2 d S . P . .
Co2 Co 0.500000 0.000000 1.000000 0.00797(17) Uani 1 2 d S . P . .
Al1 Al 0.000000 0.000000 0.500000 0.0107(3) Uani 1 2 d S . P . .
Al2 Al 1.000000 0.500000 1.000000 0.0096(3) Uani 1 2 d S . P . .
O1 O -0.0407(4) 0.2184(3) 0.5335(4) 0.0273(7) Uani 0.5 1 d D . P . .
H1A H 0.039(11) 0.288(10) 0.627(7) 0.041 Uiso 0.5 1 d D U P . .
H1B H -0.183(5) 0.216(12) 0.552(10) 0.041 Uiso 0.5 1 d D U P . .
O2 O 0.8938(4) 0.5718(3) 1.1895(3) 0.0193(6) Uani 0.5 1 d D . P . .
H2A H 0.835(14) 0.498(7) 1.242(9) 0.029 Uiso 0.5 1 d D U P . .
H2B H 0.893(15) 0.675(4) 1.259(8) 0.029 Uiso 0.5 1 d D U P . .
O3 O 0.5275(5) 0.3286(4) 0.6242(4) 0.0293(8) Uani 1 1 d D . . . .
H3A H 0.586(8) 0.351(6) 0.730(3) 0.044 Uiso 1 1 d D U . . .
H3B H 0.443(7) 0.229(4) 0.604(6) 0.044 Uiso 1 1 d D U . . .
O4 O 0.2194(4) 0.3727(3) 0.3695(3) 0.0159(6) Uani 1 1 d D . . . .
H4A H 0.118(6) 0.321(5) 0.415(5) 0.024 Uiso 1 1 d D U . . .
H4B H 0.156(6) 0.367(5) 0.268(3) 0.024 Uiso 1 1 d D U . . .
O5 O 0.3207(4) 0.6267(3) 0.6607(3) 0.0229(7) Uani 1 1 d D . . . .
H5A H 0.244(7) 0.674(5) 0.592(5) 0.034 Uiso 1 1 d D U . . .
H5B H 0.389(7) 0.698(5) 0.751(4) 0.034 Uiso 1 1 d D U . . .
O6 O 0.1849(4) -0.0697(3) 0.9223(3) 0.0164(6) Uani 1 1 d D . . . .
H6A H 0.110(6) -0.033(5) 0.845(4) 0.025 Uiso 1 1 d D U . . .
H6B H 0.105(6) -0.155(4) 0.944(5) 0.025 Uiso 1 1 d D U . . .
O7 O 0.5542(4) -0.0356(3) 0.7662(3) 0.0160(6) Uani 1 1 d D . . . .
H7A H 0.460(5) 0.008(5) 0.704(5) 0.024 Uiso 1 1 d D U . . .
H7B H 0.686(4) -0.036(5) 0.735(5) 0.024 Uiso 1 1 d D U . . .
O8 O 0.4546(4) 0.2384(3) 1.0174(3) 0.0173(6) Uani 1 1 d D . . . .
H8A H 0.323(4) 0.275(5) 1.013(5) 0.026 Uiso 1 1 d D U . . .
H8B H 0.549(5) 0.300(5) 0.976(5) 0.026 Uiso 1 1 d D U . . .
F1 F -0.0407(4) 0.2184(3) 0.5335(4) 0.0273(7) Uani 0.5 1 d . . P . .
F2 F 0.8938(4) 0.5718(3) 1.1895(3) 0.0193(6) Uani 0.5 1 d . . P . .
F3 F 0.0555(4) 0.0003(4) 0.3072(3) 0.0280(6) Uani 1 1 d . . . . .
F4 F 0.2734(3) 0.0591(3) 0.5748(3) 0.0158(5) Uani 1 1 d . . . . .
F5 F 0.7447(3) 0.3977(3) 0.9098(3) 0.0161(5) Uani 1 1 d . . . . .
F6 F 0.9308(3) 0.6758(3) 0.9408(3) 0.0153(5) 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'
Co Co 0.3494 0.9721 '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
O3 Co1 O3 180.0 2_666 . ?
O3 Co1 O4 90.40(11) 2_666 2_666 ?
O3 Co1 O4 89.60(11) . 2_666 ?
O3 Co1 O4 89.59(11) 2_666 . ?
O3 Co1 O4 90.41(11) . . ?
O4 Co1 O4 180.0 2_666 . ?
O3 Co1 O5 88.31(14) 2_666 . ?
O3 Co1 O5 91.69(14) . . ?
O4 Co1 O5 91.90(11) 2_666 . ?
O4 Co1 O5 88.10(11) . . ?
O3 Co1 O5 91.69(14) 2_666 2_666 ?
O3 Co1 O5 88.31(14) . 2_666 ?
O4 Co1 O5 88.10(11) 2_666 2_666 ?
O4 Co1 O5 91.90(11) . 2_666 ?
O5 Co1 O5 180.0 . 2_666 ?
O6 Co2 O6 180.00(5) . 2_657 ?
O6 Co2 O7 90.42(11) . 2_657 ?
O6 Co2 O7 89.58(11) 2_657 2_657 ?
O6 Co2 O7 89.58(11) . . ?
O6 Co2 O7 90.42(11) 2_657 . ?
O7 Co2 O7 180.0 2_657 . ?
O6 Co2 O8 90.19(11) . . ?
O6 Co2 O8 89.81(11) 2_657 . ?
O7 Co2 O8 87.83(11) 2_657 . ?
O7 Co2 O8 92.17(11) . . ?
O6 Co2 O8 89.81(11) . 2_657 ?
O6 Co2 O8 90.19(11) 2_657 2_657 ?
O7 Co2 O8 92.17(11) 2_657 2_657 ?
O7 Co2 O8 87.83(11) . 2_657 ?
O8 Co2 O8 180.00(2) . 2_657 ?
F3 Al1 F3 180.0 . 2_556 ?
F3 Al1 F4 90.53(10) . 2_556 ?
F3 Al1 F4 89.47(10) 2_556 2_556 ?
F3 Al1 F4 89.47(10) . . ?
F3 Al1 F4 90.53(10) 2_556 . ?
F4 Al1 F4 180.0 2_556 . ?
F3 Al1 O1 91.07(13) . 2_556 ?
F3 Al1 O1 88.93(13) 2_556 2_556 ?
F4 Al1 O1 89.51(10) 2_556 2_556 ?
F4 Al1 O1 90.49(10) . 2_556 ?
F3 Al1 O1 88.93(13) . . ?
F3 Al1 O1 91.07(13) 2_556 . ?
F4 Al1 O1 90.49(10) 2_556 . ?
F4 Al1 O1 89.51(10) . . ?
O1 Al1 O1 180.0 2_556 . ?
F5 Al2 F5 180.0 2_767 . ?
F5 Al2 F6 89.51(10) 2_767 2_767 ?
F5 Al2 F6 90.49(10) . 2_767 ?
F5 Al2 F6 90.49(10) 2_767 . ?
F5 Al2 F6 89.51(10) . . ?
F6 Al2 F6 180.0 2_767 . ?
F5 Al2 O2 90.41(11) 2_767 . ?
F5 Al2 O2 89.59(11) . . ?
F6 Al2 O2 90.25(11) 2_767 . ?
F6 Al2 O2 89.75(11) . . ?
F5 Al2 O2 89.59(11) 2_767 2_767 ?
F5 Al2 O2 90.41(11) . 2_767 ?
F6 Al2 O2 89.75(11) 2_767 2_767 ?
F6 Al2 O2 90.25(11) . 2_767 ?
O2 Al2 O2 180.0 . 2_767 ?
Al1 O1 H1A 115(6) . . ?
Al1 O1 H1B 102(6) . . ?
H1A O1 H1B 105(4) . . ?
Al2 O2 H2A 121(5) . . ?
Al2 O2 H2B 134(5) . . ?
H2A O2 H2B 105(4) . . ?
Co1 O3 H3A 124(3) . . ?
Co1 O3 H3B 127(3) . . ?
H3A O3 H3B 105(3) . . ?
Co1 O4 H4A 123(3) . . ?
Co1 O4 H4B 131(3) . . ?
H4A O4 H4B 105(3) . . ?
Co1 O5 H5A 98(3) . . ?
Co1 O5 H5B 119(3) . . ?
H5A O5 H5B 114(4) . . ?
Co2 O6 H6A 123(3) . . ?
Co2 O6 H6B 125(3) . . ?
H6A O6 H6B 110(3) . . ?
Co2 O7 H7A 114(3) . . ?
Co2 O7 H7B 124(3) . . ?
H7A O7 H7B 113(3) . . ?
Co2 O8 H8A 124(3) . . ?
Co2 O8 H8B 118(3) . . ?
H8A O8 H8B 111(3) . . ?
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
Co1 O3 2.055(3) 2_666 ?
Co1 O3 2.055(3) . ?
Co1 O4 2.083(2) 2_666 ?
Co1 O4 2.083(2) . ?
Co1 O5 2.099(3) . ?
Co1 O5 2.099(3) 2_666 ?
Co2 O6 2.051(2) . ?
Co2 O6 2.051(2) 2_657 ?
Co2 O7 2.081(3) 2_657 ?
Co2 O7 2.081(3) . ?
Co2 O8 2.085(3) . ?
Co2 O8 2.085(3) 2_657 ?
Al1 F3 1.776(2) . ?
Al1 F3 1.776(2) 2_556 ?
Al1 F4 1.788(2) 2_556 ?
Al1 F4 1.788(2) . ?
Al1 O1 1.892(3) 2_556 ?
Al1 O1 1.892(3) . ?
Al2 F5 1.791(2) 2_767 ?
Al2 F5 1.791(2) . ?
Al2 F6 1.802(2) 2_767 ?
Al2 F6 1.802(2) . ?
Al2 O2 1.866(2) . ?
Al2 O2 1.866(2) 2_767 ?
O1 H1A 0.95(2) . ?
O1 H1B 0.95(2) . ?
O2 H2A 0.95(2) . ?
O2 H2B 0.95(2) . ?
O3 H3A 0.933(19) . ?
O3 H3B 0.94(2) . ?
O4 H4A 0.945(19) . ?
O4 H4B 0.928(19) . ?
O5 H5A 0.931(19) . ?
O5 H5B 0.916(19) . ?
O6 H6A 0.927(19) . ?
O6 H6B 0.933(19) . ?
O7 H7A 0.934(19) . ?
O7 H7B 0.927(19) . ?
O8 H8A 0.931(19) . ?
O8 H8B 0.937(19) . ?
