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_7243887
_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            'C42 H86 Ag2 Mo8 N8 O26'
_chemical_formula_weight         2102.44
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5214(4)
_cell_length_b                   16.1843(4)
_cell_length_c                   23.4644(6)
_cell_measurement_reflns_used    9860
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.6010
_cell_measurement_theta_min      2.5650
_cell_volume                     6653.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'ShelXle (H\"ubschle, 2011)'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6168
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.881
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29815
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.881
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         28.950
_diffrn_reflns_theta_min         2.089
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.108
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81888
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            light-yellow
_exptl_crystal_density_diffrn    2.099
_exptl_crystal_description       block
_exptl_crystal_F_000             4128
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         7762
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0238
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0188P)^2^+3.3072P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0471
_refine_ls_wR_factor_ref         0.0505
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6429
_reflns_number_total             7762
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            d1ce01152a2.cif
_cod_data_source_block           YP
_cod_depositor_comments
'Adding full bibliography for 7243886--7243888.cif.'
_cod_database_code               7243887
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.486
_shelx_estimated_absorpt_t_max   0.678
_shelx_res_checksum              97642