Solvatomorphs of (Bu4N)2[{Ag(N2-py)}2Mo8O26]: structure, colouration and phase transition
Abramov, Pavel A.; Komarov, Vladislav Yu.; Pischur, Denis A.; Sulyaeva, Veronica S.; Benassi, Enrico; Sokolov, Maxim N.; CrystEngComm 23 (2021) 8527–8537; doi:10.1039/D1CE01152A

data_7243888
_publ_section_title
;
 Solvatomorphs of (Bu4N)2[{Ag(N2-py)}2Mo8O26]: structure, colouration and
 phase transition
;
_journal_issue                   48
_journal_name_full               CrystEngComm
_journal_page_first              8527
_journal_page_last               8537
_journal_paper_doi               10.1039/D1CE01152A
_journal_volume                  23
_journal_year                    2021
_chemical_formula_sum            'C45 H93 Ag2 Mo8 N9 O27'
_chemical_formula_weight         2175.54
_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_method           SHELXL-2017/1
_audit_update_record
;
2021-08-25 deposited with the CCDC.	2021-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                88.1980(10)
_cell_angle_beta                 74.2950(10)
_cell_angle_gamma                68.9620(10)
_cell_formula_units_Z            2
_cell_length_a                   12.9493(7)
_cell_length_b                   16.7502(5)
_cell_length_c                   18.0160(9)
_cell_measurement_reflns_used    3673
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.3074
_cell_measurement_theta_min      2.3549
_cell_volume                     3501.7(3)
_computing_cell_refinement       'SAINT (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT (Bruker-AXS, 2016)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 PIXEL
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III area detector'
_diffrn_measured_fraction_theta_full 0.937
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Incoatec HELIOS multilayer mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1007
_diffrn_reflns_av_unetI/netI     0.1230
_diffrn_reflns_Laue_measured_fraction_full 0.937
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            46874
_diffrn_reflns_point_group_measured_fraction_full 0.937
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         28.706
_diffrn_reflns_theta_min         2.355
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_exptl_absorpt_coefficient_mu    2.008
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6798
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.063
_exptl_crystal_description       block
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.098
_exptl_crystal_size_mid          0.042
_exptl_crystal_size_min          0.023
_refine_diff_density_max         1.793
_refine_diff_density_min         -1.929
_refine_diff_density_rms         0.230
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     810
_refine_ls_number_reflns         16666
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.1062
_refine_ls_R_factor_gt           0.0694
_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^)+(0.0429P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1466
_refine_ls_wR_factor_ref         0.1824
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10696
_reflns_number_total             16666
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01152a2.cif
_cod_data_source_block           OP_150
_cod_depositor_comments
'Adding full bibliography for 7243886--7243888.cif.'
_cod_database_code               7243888
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.828
_shelx_estimated_absorpt_t_max   0.955
_shelx_res_checksum              27952