Isostructural mesoporous ionic crystals as a tunable platform for acid catalysis.
Shimoyama, Yuto; Weng, Zhewei; Ogiwara, Naoki; Kitao, Takashi; Kikukawa, Yuji; Uchida, Sayaka; Dalton transactions (Cambridge, England : 2003) 49 (2020) 10328–10333; doi:10.1039/d0dt01202e

data_7704621
_publ_section_title
;
 Isostructural mesoporous ionic crystals as a tunable platform for acid
 catalysis.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10328
_journal_page_last               10333
_journal_paper_doi               10.1039/d0dt01202e
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         '2(Mo12 O40 P), 3(C18 H18 Cr3 N6 O16)'
_chemical_formula_sum            'C54 H54 Cr9 Mo24 N18 O128 P2'
_chemical_formula_weight         5835.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2020-05-31
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-06-01 deposited with the CCDC.	2020-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.351(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   57.570(16)
_cell_length_b                   24.215(7)
_cell_length_c                   18.769(5)
_cell_measurement_reflns_used    41720
_cell_measurement_temperature    163.0
_cell_measurement_theta_max      31.32
_cell_measurement_theta_min      1.83
_cell_volume                     25458(12)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97  (Sheldrick, 2008)'
_diffrn_ambient_temperature      163.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku Saturn70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0880
_diffrn_reflns_av_unetI/netI     0.0775
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       70
_diffrn_reflns_limit_h_min       -70
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            79559
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.682
_diffrn_source                   'rotating anode X-ray generator'
_exptl_absorpt_coefficient_mu    1.590
_exptl_absorpt_correction_T_max  0.718
_exptl_absorpt_correction_T_min  0.463
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            yellow-green
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             11128
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: water'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.985
_refine_diff_density_min         -1.151
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1065
_refine_ls_number_reflns         24885
_refine_ls_number_restraints     2480
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_gt           0.0665
_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^)+(0.0754P)^2^+117.7249P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1669
_refine_ls_wR_factor_ref         0.1775
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19956
_reflns_number_total             24885
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01202e2.cif
_cod_data_source_block           shelxl_sq
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7704621.cif.

 Adding full bibliography for 7704621.cif.
;
_cod_original_cell_volume        25459(12)
_cod_database_code               7704621
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.832
_shelx_estimated_absorpt_t_min   0.742
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All O(H,H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H11C(0.5) H11D(0.5)
6.a Rotating group:
 O101(H10A,H10B), O102(H10C,H10D), O103(H10E,H10F), O117(H11C,H11D), O118(H11E,
 H11F)
6.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C5(H5A,H5B), C8(H8A,H8B), C11(H11A,H11B), C14(H14A,H14B),
 C17(H17A,H17B), C20(H20A,H20B), C23(H23A,H23B), C26(H26A,H26B)
;
_shelx_res_checksum              15642
_shelx_fab_checksum              39255
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'