#------------------------------------------------------------------------------
#$Date: 2024-08-05 20:19:48 +0300 (Mon, 05 Aug 2024) $
#$Revision: 293677 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/32/7133233.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_7133233
loop_
_publ_author_name
'El Alouani Dahmouni, Nadia'
'Orts-Arroyo, Marta'
'Sanchis-Perucho, Adrián'
'Moliner, Nicolás'
'Mayans, Júlia'
'Pacheco, Mario'
'Castro, Isabel'
'De Munno, Giovanni'
'Marino, Nadia'
'Ruiz-García, Rafael'
'Martínez-Lillo, José'
_publ_section_title
;
 Magnetocaloric efficiency tuning through solvent-triggered 3D to 2D
 interconversion in holmium(III)-based dynamic MOFs.
;
_journal_issue                   58
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7451
_journal_page_last               7454
_journal_paper_doi               10.1039/d4cc02539c
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C6 H12 Ho2 O18, 4(H2 O)'
_chemical_formula_sum            'C6 H20 Ho2 O22'
_chemical_formula_weight         774.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-04-29 deposited with the CCDC.	2024-06-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.1430(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.9347(3)
_cell_length_b                   9.6040(3)
_cell_length_c                   9.9542(3)
_cell_measurement_reflns_used    9964
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.74
_cell_measurement_theta_min      2.94
_cell_volume                     953.92(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'CRYSTAL MAKER, DIAMOND'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14424
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.744
_diffrn_reflns_theta_min         2.944
_exptl_absorpt_coefficient_mu    8.344
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6297
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS'
_exptl_crystal_colour            'PALE YELLOW'
_exptl_crystal_density_diffrn    2.695
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.049
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       0.00070(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2469
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0166
_refine_ls_R_factor_gt           0.0146
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0134P)²+1.0920P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0364
_refine_ls_wR_factor_ref         0.0378
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2306
_reflns_number_total             2469
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4cc02539c2.cif
_cod_data_source_block           olmio3
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_primary' value 'Direct' was changed
to 'direct' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_atom_sites_solution_secondary' value 'Difmap' was changed
to 'difmap' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7133232--7133233.cif.
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7133233
_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   0.460
_shelx_estimated_absorpt_t_max   0.685
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, 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_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
Ho1 Ho 0.69080(2) 0.45752(2) 0.33094(2) 0.01262(5) Uani 1 1 d . . . . .
C1 C 0.4449(3) 0.5261(3) 0.4274(3) 0.0181(4) Uani 1 1 d . U . . .
O1 O 0.4739(2) 0.5261(2) 0.3172(2) 0.0213(4) Uani 1 1 d . U . . .
O2 O 0.3371(2) 0.5629(2) 0.4306(2) 0.0265(4) Uani 1 1 d . U . . .
C2 C 0.9994(2) 0.4471(2) 0.5577(3) 0.0150(4) Uani 1 1 d . U . . .
O3 O 0.88933(18) 0.3916(2) 0.5351(2) 0.0212(4) Uani 1 1 d . U . . .
O4 O 1.10876(18) 0.4262(2) 0.6644(2) 0.0206(4) Uani 1 1 d . U . . .
C3 C 0.5330(2) 0.5714(2) 0.0024(3) 0.0160(4) Uani 1 1 d . U . . .
O5 O 0.6278(2) 0.6032(2) 0.1216(2) 0.0232(4) Uani 1 1 d . U . . .
O6 O 0.48729(18) 0.64298(19) -0.11252(19) 0.0188(3) Uani 1 1 d . U . . .
O1W O 0.7105(2) 0.6867(2) 0.4276(3) 0.0328(5) Uani 1 1 d D . . . .
H1WA H 0.779(3) 0.728(4) 0.505(4) 0.049 Uiso 1 1 d D U . . .
H1WB H 0.638(3) 0.744(4) 0.420(4) 0.049 Uiso 1 1 d D U . . .
O2W O 0.7953(2) 0.3202(2) 0.2016(3) 0.0313(5) Uani 1 1 d D . . . .
H2WA H 0.8852(19) 0.324(4) 0.229(5) 0.047 Uiso 1 1 d D U . . .
H2WB H 0.775(4) 0.228(2) 0.181(4) 0.047 Uiso 1 1 d D U . . .
O3W O 0.6644(3) 0.2209(2) 0.3812(2) 0.0348(5) Uani 1 1 d D . . . .
H3WA H 0.713(4) 0.176(4) 0.468(3) 0.052 Uiso 1 1 d D U . . .
H3WB H 0.614(4) 0.153(3) 0.319(3) 0.052 Uiso 1 1 d D U . . .
O4W O 1.1009(18) 0.988(2) 0.549(3) 0.248(13) Uani 0.5 1 d . . P . .
O5W O 0.8524(16) 0.8958(16) 0.320(2) 0.216(12) Uani 0.5 1 d . . P . .
O6W O 0.9415(8) 0.7862(18) 0.6267(14) 0.162(7) Uani 0.5 1 d . . P . .
O7W O 0.9222(6) 0.6750(8) 0.7189(9) 0.0565(18) Uani 0.5 1 d . . P . .
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'
Ho Ho -0.2175 4.6783 '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'
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
O5 Ho1 O3W 137.41(7) . . ?
O5 Ho1 O3 138.29(6) . . ?
O3W Ho1 O3 73.20(7) . . ?
O5 Ho1 O1W 75.79(8) . . ?
O3W Ho1 O1W 143.27(9) . . ?
O3 Ho1 O1W 90.03(8) . . ?
O5 Ho1 O1 82.12(7) . . ?
O3W Ho1 O1 94.15(8) . . ?
O3 Ho1 O1 130.96(7) . . ?
O1W Ho1 O1 72.19(7) . . ?
O5 Ho1 O2W 83.40(8) . . ?
O3W Ho1 O2W 73.47(9) . . ?
O3 Ho1 O2W 81.10(7) . . ?
O1W Ho1 O2W 137.11(8) . . ?
O1 Ho1 O2W 141.54(7) . . ?
O5 Ho1 O4 71.47(6) . 3_766 ?
O3W Ho1 O4 128.31(8) . 3_766 ?
O3 Ho1 O4 66.84(6) . 3_766 ?
O1W Ho1 O4 68.71(7) . 3_766 ?
O1 Ho1 O4 136.90(7) . 3_766 ?
O2W Ho1 O4 69.24(7) . 3_766 ?
O5 Ho1 O6 67.15(6) . 3_665 ?
O3W Ho1 O6 71.81(7) . 3_665 ?
O3 Ho1 O6 140.55(7) . 3_665 ?
O1W Ho1 O6 129.25(7) . 3_665 ?
O1 Ho1 O6 69.53(7) . 3_665 ?
O2W Ho1 O6 72.00(7) . 3_665 ?
O4 Ho1 O6 125.37(6) 3_766 3_665 ?
O5 Ho1 O2 140.44(7) . 3_666 ?
O3W Ho1 O2 69.81(8) . 3_666 ?
O3 Ho1 O2 66.03(7) . 3_666 ?
O1W Ho1 O2 73.53(8) . 3_666 ?
O1 Ho1 O2 65.15(6) . 3_666 ?
O2W Ho1 O2 136.12(8) . 3_666 ?
O4 Ho1 O2 118.08(7) 3_766 3_666 ?
O6 Ho1 O2 116.55(7) 3_665 3_666 ?
O2 C1 O1 126.9(2) . . ?
O2 C1 C1 117.0(3) . 3_666 ?
O1 C1 C1 116.0(3) . 3_666 ?
C1 O1 Ho1 122.84(16) . . ?
C1 O2 Ho1 118.88(17) . 3_666 ?
O4 C2 O3 126.9(2) . . ?
O4 C2 C2 116.4(3) . 3_766 ?
O3 C2 C2 116.7(3) . 3_766 ?
C2 O3 Ho1 121.07(16) . . ?
C2 O4 Ho1 118.81(16) . 3_766 ?
O6 C3 O5 126.7(2) . . ?
O6 C3 C3 117.0(3) . 3_665 ?
O5 C3 C3 116.3(3) . 3_665 ?
C3 O5 Ho1 121.30(16) . . ?
C3 O6 Ho1 118.10(15) . 3_665 ?
Ho1 O1W H1WA 130(2) . . ?
Ho1 O1W H1WB 125(2) . . ?
H1WA O1W H1WB 101(2) . . ?
Ho1 O2W H2WA 120(3) . . ?
Ho1 O2W H2WB 121(3) . . ?
H2WA O2W H2WB 104(2) . . ?
Ho1 O3W H3WA 125(2) . . ?
Ho1 O3W H3WB 129(2) . . ?
H3WA O3W H3WB 105(2) . . ?
O4W O5W O7W 134.7(14) 3_776 4_575 ?
O6W O7W O5W 154.4(8) . 4_576 ?
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
Ho1 O5 2.3663(18) . ?
Ho1 O3W 2.369(2) . ?
Ho1 O3 2.3739(18) . ?
Ho1 O1W 2.376(2) . ?
Ho1 O1 2.4108(19) . ?
Ho1 O2W 2.430(2) . ?
Ho1 O4 2.4434(19) 3_766 ?
Ho1 O6 2.4469(18) 3_665 ?
Ho1 O2 2.522(2) 3_666 ?
C1 O2 1.243(3) . ?
C1 O1 1.260(3) . ?
C1 C1 1.539(5) 3_666 ?
C2 O4 1.249(3) . ?
C2 O3 1.250(3) . ?
C2 C2 1.537(5) 3_766 ?
C3 O6 1.251(3) . ?
C3 O5 1.253(3) . ?
C3 C3 1.541(5) 3_665 ?
O1W H1WA 0.914(18) . ?
O1W H1WB 0.940(18) . ?
O2W H2WA 0.907(18) . ?
O2W H2WB 0.920(18) . ?
O3W H3WA 0.918(18) . ?
O3W H3WB 0.916(18) . ?
O4W O5W 1.63(3) 3_776 ?
O5W O7W 1.63(3) 4_575 ?
O6W O7W 1.479(18) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1W H1WA O6W 0.914(18) 1.79(2) 2.669(8) 162(4) . yes
O1W H1WB O6 0.940(18) 1.890(18) 2.828(3) 175(4) 4_576 yes
O2W H2WA O7W 0.907(18) 1.95(2) 2.859(7) 177(4) 3_766 yes
O2W H2WB O2 0.920(18) 2.03(2) 2.895(3) 156(4) 2_645 yes
O3W H3WA O2W 0.918(18) 2.12(3) 2.940(3) 148(4) 4_566 yes
O3W H3WB O1 0.916(18) 1.780(19) 2.691(3) 173(4) 2_645 yes
