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_7131288
_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), 1.75[C8H9NO]'
_chemical_formula_sum            'C86 H75.75 Mo12 N1.75 O41.75 P4'
_chemical_formula_weight         3076.89
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-01-30
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2023.01.20 svn.r024a95a1 for OlexSys, GUI svn.r6444)
;
_audit_update_record
;
2023-02-10 deposited with the CCDC.	2023-02-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.437(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.219(3)
_cell_length_b                   25.074(6)
_cell_length_c                   27.423(7)
_cell_measurement_reflns_used    9634
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.36
_cell_volume                     9695(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       APEX2(Bruker,2014)
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip  (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1447
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            317477
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.105
_exptl_absorpt_coefficient_mu    1.653
_exptl_absorpt_correction_T_max  0.0962
_exptl_absorpt_correction_T_min  0.0638
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1105 before and 0.0997 after correction.
The Ratio of minimum to maximum transmission is 0.6632.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.108
_exptl_crystal_description       plate
_exptl_crystal_F_000             6008
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of water and methanol  by slow evaporation'
_exptl_crystal_size_max          0.195
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.175
_refine_diff_density_max         1.107
_refine_diff_density_min         -1.129
_refine_diff_density_rms         0.140
_refine_ls_extinction_coef       0.000103(14)
_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   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1190
_refine_ls_number_reflns         17041
_refine_ls_number_restraints     360
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0530
_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^)+(0.0186P)^2^+101.7787P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1104
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12616
_reflns_number_total             17041
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03273b2.cif
_cod_data_source_block           comp-2_sg
_cod_depositor_comments
'Adding full bibliography for 7131286--7131288.cif.'
_cod_database_code               7131288
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.761
_shelx_estimated_absorpt_t_min   0.739
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C69) \\sim Ueq, Uanis(P4) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C49)
\\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C66) \\sim Ueq,
Uanis(C62) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C60)
\\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C68) \\sim Ueq,
Uanis(C65) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C53)
\\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C71) \\sim Ueq,
Uanis(C64) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C70)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O8) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O4) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 P4, C61, C49, C55, C67, C66, C62, C50, C54, C60, C56, C72, C68, C65, C63, C51,
  C53, C52, C59, C57, C71, C69, C70, C64, C58
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: O3(0.83) O5(0.83) O7(0.83) O1(0.83) O2(0.17) O6(0.17) O8(0.17)
 O4(0.17)
5.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C18(H18), C2(H2), C41(H41), C17(H17), C20(H20), C22(H22), C42(H42),
 C38(H38), C26(H26), C36(H36), C66(H66), C3(H3), C45(H45), C4(H4), C24(H24),
 C21(H21), C63(H63), C12(H12), C32(H32), C62(H62), C35(H35), C28(H28), C8(H8),
 C34(H34), C48(H48), C9(H9), C39(H39), C46(H46), C5(H5), C27(H27), C47(H47),
 C6(H6), C30(H30), C44(H44), C15(H15), C16(H16), C29(H29), C33(H33), C23(H23),
 C11(H11), C10(H10), C65(H65), C64(H64), C40(H40), C71(H71), C60(H60), C50(H50),
  C51(H51), C53(H53), C56(H56), C54(H54), C72(H72), C68(H68), C52(H52),
 C59(H59), C58(H58), C70(H70), C57(H57), C69(H69)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 506 electrons were 
found in a volume of 1558\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 1.75[C8H9NO] per Formula Unit 
( 7*N-Methyl Formanilide per unit cell) which account for 504 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              3107
_shelx_hkl_checksum              97420
_shelx_fab_checksum              85591
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'