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_7131286
_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, 4(C24 H20 P), 3(C8 H9 N O)'
_chemical_formula_sum            'C120 H107 Mo12 N3 O43 P5'
_chemical_formula_weight         3585.21
_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             2023-01-09
_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                84.920(3)
_cell_angle_beta                 66.901(2)
_cell_angle_gamma                67.164(2)
_cell_formula_units_Z            1
_cell_length_a                   14.9244(8)
_cell_length_b                   14.9531(9)
_cell_length_c                   16.6482(9)
_cell_measurement_reflns_used    9990
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      27.669
_cell_measurement_theta_min      2.457
_cell_volume                     3140.7(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       APEX2(Bruker,2014.3-0)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      292.00
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            90355
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.457
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.304
_exptl_absorpt_correction_T_max  0.0961
_exptl_absorpt_correction_T_min  0.0660
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0725 before and 0.0497 after correction.
The Ratio of minimum to maximum transmission is 0.6868.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.896
_exptl_crystal_description       block
_exptl_crystal_F_000             1771
_exptl_crystal_recrystallization_method
'The material was recrystallised from N-Methyl Formanilide  by slow evaporation'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.205
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.831
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.133
_refine_ls_extinction_coef       0.00103(10)
_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   1.362
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     868
_refine_ls_number_reflns         10960
_refine_ls_number_restraints     512
_refine_ls_restrained_S_all      1.359
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0679
_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^)+34.5682P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1416
_refine_ls_wR_factor_ref         0.1439
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9992
_reflns_number_total             10960
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03273b2.cif
_cod_data_source_block           compound1
_cod_depositor_comments
'Adding full bibliography for 7131286--7131288.cif.'
_cod_database_code               7131286
_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
 C58-C57
 1.4 with sigma of 0.02
 C58-C59
 1.54 with sigma of 0.02
 C57-C62
 1.4 with sigma of 0.02
 C57-N2
 1.35 with sigma of 0.02
3. Rigid body (RIGU) restrains
 P1, Mo6, O11, O22, O14, O16, O12, O4, O3, Mo5, Mo2, O1, O2, O13, O21, O10, O9,
  O18, O7, O6, O15, Mo1, Mo3, Mo4, O17, O5, O19, O8, O20
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C64, C49, N1, C56, C55, C50, C54, O23, H56, H55A, H55B, H55C, H50, C51, H54,
 C53, C52, H51, H52, H53, C57, O24, N2, C63, C58, C62, C59, C61, C60
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Others
 Fixed Sof: O4(0.5) O2(0.5) O3(0.5) O24(0.5) C58(0.5) H58(0.5) C57(0.5)
 C62(0.5) H62(0.5) C61(0.5) H61(0.5) C60(0.5) H60(0.5) C59(0.5) H59(0.5)
 O1(0.5) C63(0.5) H63A(0.5) H63B(0.5) H63C(0.5) C64(0.5) H64(0.5) N2(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C44(H44), C26(H26), C45(H45), C30(H30), C27(H27), C36(H36), C23(H23),
 C32(H32), C28(H28), C33(H33), C34(H34), C8(H8), C24(H24), C48(H48), C6(H6),
 C14(H14), C46(H46), C4(H4), C42(H42), C22(H22), C15(H15), C5(H5), C41(H41),
 C20(H20), C47(H47), C38(H38), C2(H2), C29(H29), C40(H40), C10(H10), C18(H18),
 C3(H3), C11(H11), C39(H39), C16(H16), C12(H12), C9(H9), C35(H35), C52(H52),
 C51(H51), C50(H50), C54(H54), C53(H53), C17(H17), C56(H56), C21(H21), C58(H58),
  C62(H62), C61(H61), C60(H60), C59(H59), C64(H64)
5.b Fitted hexagon refined as free rotating group:
 C52(C51,C50,C49,C54,C53), C58(C57,C62,C61,C60,C59)
5.c Idealised Me refined as rotating group:
 C55(H55A,H55B,H55C), C63(H63A,H63B,H63C)
;
_shelx_res_checksum              96864
_shelx_hkl_checksum              47319
_olex2_submission_special_instructions 'No special instructions were received'