pH-induced phase transition and crystallization of soft-oxometalates (SOMs) into polyoxometalates (POMs): a study on crystallization from colloids.
Paul, Shounik; Sreejith, S. S.; Roy, Soumyajit; Acta crystallographica. Section C, Structural chemistry 74 (2018) 1274–1283; doi:10.1107/S2053229618007143

data_2311990
_publ_section_title
;
 pH-induced phase transition and crystallization of soft-oxometalates
 (SOMs) into polyoxometalates (POMs): a study on crystallization from
 colloids.
;
_journal_coeditor_code           JR3006
_journal_issue                   'Pt 11'
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_page_first              1274
_journal_page_last               1283
_journal_paper_doi               10.1107/S2053229618007143
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          '(C6 H16 N)3 [K2 Mo16 O52]0.5, H2 O'
_chemical_formula_moiety         '3(C6 H16 N +), 0.5(K2 Mo16 O52 6-), H2 O'
_chemical_formula_sum            'C18 H50 K Mo8 N3 O27'
_chemical_formula_weight         1547.23
_chemical_name_common            '1D-octamolybdate Chain'
_chemical_name_systematic
;
Tris(triethylaminium) hemi(dopentacontaoxidopotassiohexadecamolybdate)
monohydrate
;
_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_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 121.835(3)
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_cell_length_c                   18.5442(5)
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_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      26.7990
_cell_measurement_theta_min      2.0870
_cell_volume                     4258.5(3)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
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OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100.00(10)
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_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type
'Agilent SuperNova Dual Source diffractometer with an Eos detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12607
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.205
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.463
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;
(SADABS; Bruker, 2008)
;
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_exptl_crystal_size_min          0.05
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_refine_ls_extinction_method
;
SHELXL2016 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_reflns         3886
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0229
_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^)+(0.0247P)^2^+6.8377P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0549
_refine_ls_wR_factor_ref         0.0564
_reflns_number_gt                3582
_reflns_number_total             3886
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jr3006sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        4258.5(2)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2311990
_shelx_estimated_absorpt_t_min   0.525
_shelx_estimated_absorpt_t_max   0.887