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_7243886
_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
_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                104.626(3)
_cell_angle_beta                 106.317(2)
_cell_angle_gamma                91.236(2)
_cell_formula_units_Z            4
_cell_length_a                   16.5639(8)
_cell_length_b                   17.9149(9)
_cell_length_c                   25.3059(15)
_cell_measurement_reflns_used    9742
_cell_measurement_temperature    84(2)
_cell_measurement_theta_max      29.0004
_cell_measurement_theta_min      2.3090
_cell_volume                     6938.6(6)
_computing_cell_refinement       'SAINT (Bruker-AXS, 2004)'
_computing_data_collection       'APEX2 (Bruker-AXS, 2004)'
_computing_data_reduction        'SAINT (Bruker-AXS, 2004)'
_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      84(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \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  0.0779
_diffrn_reflns_av_unetI/netI     0.0831
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            186187
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         29.591
_diffrn_reflns_theta_min         1.264
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.026
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS, 2004)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.083
_exptl_crystal_description       block
_exptl_crystal_F_000             4288
_exptl_crystal_size_max          0.098
_exptl_crystal_size_mid          0.042
_exptl_crystal_size_min          0.023
_refine_diff_density_max         3.307
_refine_diff_density_min         -2.615
_refine_diff_density_rms         0.241
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1641
_refine_ls_number_reflns         38895
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.1124
_refine_ls_R_factor_gt           0.0742
_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^)+131.5944P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1557
_refine_ls_wR_factor_ref         0.1699
_reflns_Friedel_coverage         0.000
_reflns_number_gt                26438
_reflns_number_total             38895
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            d1ce01152a2.cif
_cod_data_source_block           OP_subunit
_cod_depositor_comments
'Adding full bibliography for 7243886--7243888.cif.'
_cod_database_code               7243886
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.826
_shelx_estimated_absorpt_t_max   0.955
_shelx_res_checksum              45958