Light-induced dissolution and concomitant crystallization of a Keggin-type polyoxometalate mimicking a naturally occurring phenomenon.
Tandekar, Kesar; Schmidtmann, Marc; Tripathi, Anjali; Mishra, Neeraj Kumar; Supriya, Sabbani; Chemical communications (Cambridge, England) 59 (2023) 3241–3244; doi:10.1039/d2cc03273b

data_7131287
_publ_section_title
;
 Light-induced dissolution and concomitant crystallization of a
 Keggin-type polyoxometalate mimicking a naturally occurring phenomenon.
;
_journal_issue                   22
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3241
_journal_page_last               3244
_journal_paper_doi               10.1039/d2cc03273b
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'Mo12 O40 P, 3(C24 H20 P), 2(C8 H9 N O)'
_chemical_formula_sum            'C88 H78 Mo12 N2 O42 P4'
_chemical_formula_weight         3110.68
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-12-26
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.11.02 svn.ra8b101fa for OlexSys, GUI svn.r6635)
;
_audit_update_record
;
2023-02-10 deposited with the CCDC.	2023-02-10 downloaded from the CCDC.
;
_cell_angle_alpha                89.026(3)
_cell_angle_beta                 88.285(4)
_cell_angle_gamma                82.439(3)
_cell_formula_units_Z            2
_cell_length_a                   14.6105(11)
_cell_length_b                   15.5593(11)
_cell_length_c                   22.6072(16)
_cell_measurement_reflns_used    9580
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      28.51
_cell_measurement_theta_min      2.51
_cell_volume                     5091.9(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       APEX2(Bruker,2014)
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      292.04
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CMOS detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            215632
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.332
_diffrn_reflns_theta_min         2.221
_exptl_absorpt_coefficient_mu    1.575
_exptl_absorpt_correction_T_max  0.0961
_exptl_absorpt_correction_T_min  0.0650
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction.'
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.029
_exptl_crystal_description       plate
_exptl_crystal_F_000             3040
_exptl_crystal_recrystallization_method
'The material was recrystallised from N-Methyl Formanilide by slow evaporation'
_exptl_crystal_size_max          0.205
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.175
_refine_diff_density_max         2.002
_refine_diff_density_min         -1.696
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       0.00038(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1504
_refine_ls_number_reflns         25302
_refine_ls_number_restraints     971
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0225P)^2^+27.6915P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.1081
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18691
_reflns_number_total             25302
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03273b2.cif
_cod_data_source_block           compound3
_cod_depositor_comments
'Adding full bibliography for 7131286--7131288.cif.'
_cod_database_code               7131287
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C86-C85
 1.54 with sigma of 0.02
 C85-C86
 1.54 with sigma of 0.02
 C85-C90 \\sim C91-C96
 with sigma of 0.02
 N3-C85 \\sim N3-C91
 with sigma of 0.02
 C85-C86 \\sim C91-C92
 with sigma of 0.02
 N3-C90 \\sim N3-C96
 with sigma of 0.04
 N3-C86 \\sim N3-C92
 with sigma of 0.04
 C85-C89 \\sim C91-C95
 with sigma of 0.04
 C85-C87 \\sim C91-C93
 with sigma of 0.04
 C89-C87 \\sim C95-C93
 with sigma of 0.04
 C90-C89 \\sim C96-C95
 with sigma of 0.02
 C88-C87 \\sim C94-C93
 with sigma of 0.02
 C90-C88 \\sim C96-C94
 with sigma of 0.04
 C86-C87 \\sim C92-C93
 with sigma of 0.02
 C88-C89 \\sim C94-C95
 with sigma of 0.02
 C90-C86 \\sim C96-C92
 with sigma of 0.04
 C86-C88 \\sim C92-C94
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C88 \\sim C87: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C88 \\sim C89: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C86 \\sim C87: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
N3 \\sim C85 \\sim C86 \\sim C87 \\sim C88 \\sim C89 \\sim C90: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.02 within 2A
N3 \\sim C91 \\sim C92 \\sim C93 \\sim C94 \\sim C95 \\sim C96: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.02 within 2A
C69 \\sim N1 \\sim C73 \\sim O45 \\sim C76: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.02 within 2A
N3 \\sim C98: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.02
within 2A
Uanis(C69) \\sim Ueq: with sigma of 0.007 and sigma for terminal atoms of 0.014
Uanis(C77) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 Mo6, Mo11, O26, O27, O25, O29, O6, O43, Mo4, Mo12, Mo10, P1, O24, O14, O13,
 O36, O44, O30, O28, O32, O8, O21, O23, O42, O38, O17, O16, O3, O1, Mo5, Mo3,
 Mo9, Mo8, Mo2, Mo7, Mo1, O37, O12, O15, O35, O11, O10, O41, O22, O31, O40, O20,
  O19, O34, O9, O18, O39, O33
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C77, O46, C83, N2, H83, C84, H84A, H84B, H84C, C78, C82, H78, C79, H82, C81,
 H79, C80, H81, H80
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C91)=Sof(C96)=Sof(H96)=Sof(C95)=Sof(H95)=Sof(C94)=Sof(H94)=Sof(C93)=
 Sof(H93)=Sof(C92)=Sof(H92)=1-FVAR(1)
 Sof(C85)=Sof(C90)=Sof(H90)=Sof(C86)=Sof(H86)=Sof(C88)=Sof(H88)=Sof(C89)=
 Sof(H89)=Sof(C87)=Sof(H87)=FVAR(1)
 Fixed Sof: O8(0.8) O6(0.8) O1(0.8) O3(0.8) O45(0.5) N1(0.5) C69(0.5) C71(0.5)
 H71(0.5) C75(0.5) H75(0.5) C74(0.5) H74(0.5) C70(0.5) H70(0.5) C72(0.5)
 H72(0.5) C76(0.5) H76A(0.5) H76B(0.5) H76C(0.5) C73(0.5) H73(0.5) O46(0.5)
 N2(0.5) C84(0.5) H84A(0.5) H84B(0.5) H84C(0.5) C78(0.5) H78(0.5) C79(0.5)
 H79(0.5) C82(0.5) H82(0.5) C80(0.5) H80(0.5) C81(0.5) H81(0.5) C83(0.5)
 H83(0.5) C77(0.5) O7(0.2) O2(0.2) O5(0.2) O4(0.2)
6.a Aromatic/amide H refined with riding coordinates:
 C56(H56), C58(H58), C65(H65), C64(H64), C52(H52), C68(H68), C62(H62),
 C66(H66), C61(H61), C59(H59), C50(H50), C67(H67), C46(H46), C53(H53), C55(H55),
  C54(H54), C48(H48), C49(H49), C60(H60), C47(H47), C6(H6), C5(H5), C24(H24),
 C15(H15), C4(H4), C14(H14), C16(H16), C8(H8), C12(H12), C20(H20), C23(H23),
 C2(H2), C9(H9), C3(H3), C18(H18), C10(H10), C22(H22), C11(H11), C17(H17),
 C21(H21), C102(H102), C40(H40), C42(H42), C38(H38), C32(H32), C26(H26),
 C101(H101), C43(H43), C44(H44), C41(H41), C33(H33), C34(H34), C35(H35),
 C27(H27), C100(H100), C28(H28), C99(H99), C36(H36), C30(H30), C29(H29),
 C97(H97), C90(H90), C86(H86), C88(H88), C89(H89), C87(H87), C71(H71), C75(H75),
  C74(H74), C70(H70), C72(H72), C73(H73), C78(H78), C79(H79), C82(H82),
 C80(H80), C81(H81), C83(H83), C96(H96), C95(H95), C94(H94), C93(H93), C92(H92)
6.b Fitted hexagon refined as free rotating group:
 C91(C96,C95,C94,C93,C92)
6.c Idealised Me refined with riding coordinates:
 C76(H76A,H76B,H76C), C84(H84A,H84B,H84C)
6.d Idealised Me refined as rotating group:
 C98(H98A,H98B,H98C)
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_shelx_res_checksum              5388
_shelx_hkl_checksum              62348
_olex2_submission_special_instructions 'No special instructions were received'