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_1559746
_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
'0.5(Al12 H68 Mo72 O384 P48), 9(O), 2(C12 H11 N2), 9(C12 H12 N2)'
_chemical_formula_sum            'C132 H114 Al6 Mo36 N22 O201 P24'
_chemical_formula_weight         9583.45
_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
_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                 117.571(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   48.173(5)
_cell_length_b                   13.8607(13)
_cell_length_c                   47.347(5)
_cell_measurement_reflns_used    9535
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.964
_cell_measurement_theta_min      2.303
_cell_volume                     28024(5)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -57
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            69187
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.984
_diffrn_reflns_theta_max         24.984
_diffrn_reflns_theta_min         0.970
_exptl_absorpt_coefficient_mu    1.824
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6188
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0884 before and 0.0350 after correction.
The Ratio of minimum to maximum transmission is 0.8304.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.271
_exptl_crystal_description       block
_exptl_crystal_F_000             18472
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.339
_refine_diff_density_min         -1.698
_refine_diff_density_rms         0.197
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1921
_refine_ls_number_reflns         24556
_refine_ls_number_restraints     4052
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0594
_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/[\s^2^(Fo^2^)+(0.0378P)^2^+1211.1628P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1433
_refine_ls_wR_factor_ref         0.1485
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21199
_reflns_number_total             24556
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc05277a2.cif
_cod_data_source_block           1_sq
_cod_depositor_comments
;Adding full bibliography for 1559745--1559746.cif.

 Adding full bibliography for 1559745--1559746.cif.
;
_cod_database_code               1559746
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.735
_shelx_estimated_absorpt_t_min   0.712
_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
2. Restrained distances
 O12-H12
 0.85 with sigma of 0.01
 O21-H21
 0.85 with sigma of 0.01
 O25-H25
 0.85 with sigma of 0.01
 O33-H33
 0.85 with sigma of 0.01
 O41-H41
 0.85 with sigma of 0.01
 O44-H44
 0.85 with sigma of 0.01
 O54-H54
 0.85 with sigma of 0.01
 O58-H58
 0.85 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
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 O32 \\sim O33 \\sim O34 \\sim O35 \\sim O36
\\sim O37 \\sim O38 \\sim O39 \\sim O40 \\sim O41 \\sim O42 \\sim O43 \\sim O44
\\sim O45 \\sim O46 \\sim O47 \\sim O48 \\sim O49 \\sim O50 \\sim O51 \\sim O52
\\sim O53 \\sim O54 \\sim O55 \\sim O56 \\sim O57 \\sim O58 \\sim O59 \\sim O60
\\sim O61 \\sim O62 \\sim O63 \\sim O64 \\sim O65 \\sim O66 \\sim O67 \\sim O68
\\sim O69 \\sim O70 \\sim O71 \\sim O72 \\sim O73 \\sim O74 \\sim O75 \\sim O76
\\sim O77 \\sim O78 \\sim O79 \\sim O81 \\sim O82 \\sim O83 \\sim O84 \\sim O85
\\sim O86 \\sim O87 \\sim O88 \\sim O89 \\sim O90 \\sim O91 \\sim O92 \\sim O93
\\sim O94 \\sim O95 \\sim O96 \\sim O80 \\sim O3 \\sim O2 \\sim O1 \\sim O1W
\\sim O2W \\sim O3W \\sim O4W \\sim O5W \\sim O6W \\sim O7W \\sim C32 \\sim C31
\\sim C35 \\sim C34 \\sim C36 \\sim C8 \\sim C33 \\sim C1 \\sim C30 \\sim C7
\\sim C6 \\sim C4 \\sim C27 \\sim C28 \\sim C5 \\sim C24 \\sim C2 \\sim C57
\\sim C11 \\sim C56 \\sim C20 \\sim C3 \\sim C55 \\sim C23 \\sim C12 \\sim C9
\\sim C25 \\sim C51 \\sim C53 \\sim C18 \\sim C29 \\sim C58 \\sim C10 \\sim C60
\\sim C21 \\sim C59 \\sim C19 \\sim C54 \\sim C26 \\sim C46 \\sim C47 \\sim C15
\\sim C22 \\sim C44 \\sim C65 \\sim C52 \\sim C64 \\sim C40 \\sim C48 \\sim C39
\\sim C43 \\sim C45 \\sim C38 \\sim C63 \\sim C13 \\sim C16 \\sim C14 \\sim C49
\\sim C50 \\sim C42 \\sim C41 \\sim C37 \\sim C62 \\sim C66 \\sim C61 \\sim
C17: within 3.8A with sigma of 0.04 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: O4W(0.5) O5W(0.5) O6W(0.5) O7W(0.5) O8W(0.5)
5.a Riding coordinates:
 O12(H12), O21(H21), O25(H25), O33(H33), O41(H41), O44(H44), O54(H54), O58(H58)
5.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N6(H6), N5(H5), C31(H31), C35(H35), N4(H4), N10(H10),
 C34(H34), C36(H36), C33(H33A), C30(H30), C7(H7A), C6(H6A), C4(H4A), C28(H28),
 C5(H5A), C24(H24), C2(H2A), C11(H11), C56(H56), C55(H55), C23(H23), N3(H3),
 C12(H12A), C9(H9A), C25(H25A), C53(H53), C18(H18), C29(H29), C58(H58A),
 C10(H10A), C60(H60), C21(H21A), N9(H9), C59(H59A), C19(H19), N8(H8), C54(H54A),
  C26(H26), N11(H11A), C46(H46), C47(H47), C22(H22), C52(H52A), C64(H64),
 C40(H40), C48(H48), N7(H7), C43(H43), C45(H45), C38(H38), C63(H63), C13(H13),
 C16(H16), C14(H14), C49(H49), C50(H50), C42(H42), C41(H41A), C37(H37),
 C62(H62), C66(H66), C61(H61), C17(H17)
5.c Tetrahedral OH refined with riding coordinates:
 O52(H52), O59(H59), O84(H84), O92(H92), O93(H93), O94(H94), O95(H95),
 O96(H96), O80(H80)
;
_shelx_res_checksum              34197
_shelx_fab_checksum              35729
_olex2_submission_special_instructions 'No special instructions were received'