Stable monovalent aluminum(i) in a reduced phosphomolybdate cluster as an active acid catalyst.
Zhang, Ya-Qi; Zhou, Lai-Yun; Ma, Yuan-Yuan; Dastafkan, Kamran; Zhao, Chuan; Wang, Lan-Zhi; Han, Zhan-Gang; Chemical science 12 (2020) 1886–1890; doi:10.1039/d0sc05277a

data_1559745
_publ_section_title
;
 Stable monovalent aluminum(i) in a reduced phosphomolybdate cluster as an
 active acid catalyst.
;
_journal_issue                   5
_journal_name_full               'Chemical science'
_journal_page_first              1886
_journal_page_last               1890
_journal_paper_doi               10.1039/d0sc05277a
_journal_volume                  12
_journal_year                    2020
_chemical_formula_moiety
'Al0.5 H7 Mo6 O31 P4, 1.5(C12 H12 N2), H2 O, 2.25(O)'
_chemical_formula_sum            'C18 H18 Al0.5 Mo6 N3 O34.25 P4'
_chemical_formula_weight         1537.36
_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   mixed
_audit_creation_date             2020-08-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-11-08 deposited with the CCDC.	2020-12-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.203(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.438(2)
_cell_length_b                   23.034(4)
_cell_length_c                   15.788(3)
_cell_measurement_reflns_used    9946
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.22
_cell_measurement_theta_min      2.29
_cell_volume                     4142.4(13)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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    'Bruker SHELXTL'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20630
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.008
_diffrn_reflns_theta_max         25.008
_diffrn_reflns_theta_min         1.568
_exptl_absorpt_coefficient_mu    2.042
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.465
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             2958
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.684
_refine_diff_density_min         -0.899
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         7293
_refine_ls_number_restraints     1197
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0339
_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^)+(0.0363P)^2^+22.7508P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0878
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6435
_reflns_number_total             7293
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc05277a2.cif
_cod_data_source_block           9
_cod_depositor_comments
;Adding full bibliography for 1559745--1559746.cif.

 Adding full bibliography for 1559745--1559746.cif.
;
_cod_original_cell_volume        4142.3(13)
_cod_original_formula_sum        'C18 H18 Al0.50 Mo6 N3 O34.25 P4'
_cod_database_code               1559745
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.640
_shelx_estimated_absorpt_t_min   0.579
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 C17-C18
 1.4 with sigma of 0.02
 C18B-C17B
 1.4 with sigma of 0.02
 C8-C17
 1.5 with sigma of 0.02
 C18-C3
 1.5 with sigma of 0.02
 C17B-C8
 1.5 with sigma of 0.02
 C18B-C3
 1.5 with sigma of 0.02
 O9-H9
 0.85 with sigma of 0.01
 O4-H4
 0.85 with sigma of 0.01
 O11-H11
 0.85 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C18B \\sim C17B: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.02
O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7 \\sim O8 \\sim O9
\\sim O10 \\sim O11 \\sim O12 \\sim O13 \\sim O14 \\sim O15 \\sim O16 \\sim O17
\\sim O18 \\sim O19 \\sim O20 \\sim O21 \\sim O22 \\sim O23 \\sim O24 \\sim O25
\\sim O26 \\sim O27 \\sim O28 \\sim O29 \\sim O30 \\sim O31 \\sim O1A \\sim O2W
\\sim O3W \\sim O4W \\sim O31B \\sim O30B: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O4W) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(O30) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: O30(0.7) O31(0.5) H31(0.5) C17(0.5) H17(0.5) C18(0.5) H18(0.5)
 O3W(0.75) C18B(0.5) H18B(0.5) C17B(0.5) H17B(0.5) O4W(0.5) O31B(0.5) H2(0.5)
 O30B(0.3)
5.a Riding coordinates:
 O4(H4), O9(H9), O11(H11)
5.b Free rotating group:
 O1A(H1AA,H1AB)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2A), C4(H4A), C5(H5), C6(H6), C7(H7), C9(H9A), C10(H10),
 C11(H11A), C12(H12), C14(H14), C15(H15), C16(H16), N1(H1A), N2(H2B), N3(H3),
 C17(H17), C18(H18), C18B(H18B), C17B(H17B)
5.d Tetrahedral OH refined with riding coordinates:
 O19(H19), O22(H22), O28(H28), O31(H31), O31B(H2)
;
_shelx_res_checksum              69951
_olex2_submission_special_instructions 'No special instructions were received'