Designed synthesis of a proton-conductive Ho-MOF with reversible dehydration and hydration.
Wang, Sa-Sa; Wu, Xiao-Yuan; Li, Zhong; Lu, Can-Zhong; Dalton transactions (Cambridge, England : 2003) 48 (2019) 9930–9934; doi:10.1039/c9dt02269d

data_7700256
_publ_section_title
;
 Designed synthesis of a proton-conductive Ho-MOF with reversible
 dehydration and hydration.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9930
_journal_page_last               9934
_journal_paper_doi               10.1039/c9dt02269d
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C8 H13 Ho O12 S, 3(H2 O)'
_chemical_formula_sum            'C8 H19 Ho O15 S'
_chemical_formula_weight         552.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-12-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-19 deposited with the CCDC.    2019-05-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.273(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4135(3)
_cell_length_b                   10.5485(3)
_cell_length_c                   17.0809(4)
_cell_measurement_reflns_used    3061
_cell_measurement_temperature    100.00(13)
_cell_measurement_theta_max      70.0560
_cell_measurement_theta_min      4.9640
_cell_volume                     1663.38(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2083
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -20.00  38.00   1.00    1.00    --    0.00  57.00 -30.00   58
  2  \w     10.00  68.00   1.00    1.00    --    0.00  57.00  30.00   58
  3  \w     44.00 107.00   1.00    1.00    --   54.00-125.00 150.00   63
  4  \w    -14.00  14.00   1.00    1.00    --   54.00 -77.00  90.00   28
  5  \w     59.00  84.00   1.00    1.00    --   54.00 -77.00  90.00   25
  6  \w     25.00 119.00   1.00    1.00    --   54.00  77.00-150.00   94
  7  \w      5.00  71.00   1.00    1.00    --   54.00 -57.00-120.00   66
  8  \w     47.00 112.00   1.00    1.00    --  108.00-111.00  90.00   65
  9  \w    103.00 146.00   1.00    1.00    --  108.00 111.00-150.00   43
 10  \w     87.00 176.00   1.00    1.00    --  108.00  63.00 -90.00   89
 11  \w    101.00 151.00   1.00    1.00    --  108.00 111.00 -30.00   50
 12  \w     57.00 106.00   1.00    1.00    --  108.00-111.00   0.00   49
 13  \w    138.00 177.00   1.00    1.00    --  108.00 111.00 -90.00   39
 14  \w    105.00 132.00   1.00    1.00    --  108.00 111.00 -90.00   27
 15  \w     66.00 113.00   1.00    1.00    --  108.00-111.00-150.00   47
 16  \w    129.00 173.00   1.00    1.00    --  108.00 111.00-120.00   44
 17  \w     40.00 123.00   1.00    1.00    --  108.00 -63.00-180.00   83
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0148753000
_diffrn_orient_matrix_UB_12      0.1367858000
_diffrn_orient_matrix_UB_13      -0.0323051000
_diffrn_orient_matrix_UB_21      0.1587216000
_diffrn_orient_matrix_UB_22      -0.0028261000
_diffrn_orient_matrix_UB_23      -0.0105395000
_diffrn_orient_matrix_UB_31      -0.0490255000
_diffrn_orient_matrix_UB_32      -0.0511542000
_diffrn_orient_matrix_UB_33      -0.0854969000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6023
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.595
_diffrn_reflns_theta_max         66.595
_diffrn_reflns_theta_min         4.955
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.812
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52040
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.205
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         2935
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0288
_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/[\s^2^(Fo^2^)+(0.0466P)^2^+0.4965P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0782
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2674
_reflns_number_total             2935
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02269d2.cif
_cod_data_source_block           518-ho
_cod_depositor_comments          'Adding full bibliography for 7700256.cif.'
_cod_original_cell_volume        1663.39(8)
_cod_database_code               7700256
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C O S H Ho'
_shelx_estimated_absorpt_t_max   0.614
_shelx_estimated_absorpt_t_min   0.221
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.29
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H12A,H12B} of O12, {H10A,H10B} of O10, {H9A,H9B} of O9,
  {H8A,H8B} of O8, {H11A,H11B} of O11, {H15A,H15B} of O15, {H13A,H13B} of O13
 At 1.5 times of:
  {H14A,H14B} of O14
2.a Riding coordinates:
 O8(H8A,H8B), O9(H9A,H9B), O10(H10A,H10B), O11(H11A,H11B), O12(H12A,H12B),
 O13(H13A,H13B), O15(H15A,H15B)
2.b Free rotating group:
 O14(H14A,H14B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6)
;
_shelx_res_checksum              30807
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.924
_oxdiff_exptl_absorpt_empirical_full_min 0.727