Reentrant structural and optical properties of organic–inorganic hybrid metal cluster compound ((n-C4H9)4N)2[Mo6Bri8Bra6]
Saito, Norio; Nishiyama, Daiki; Matsushita, Yoshitaka; Wada, Yoshiki; Cordier, Stéphane; Ohsawa, Takeo; Grasset, Fabien; Ohashi, Naoki; CrystEngComm 24 (2022) 465–470; doi:10.1039/D1CE01033F

data_7244017
_publ_section_title
;
 Reentrant structural and optical properties of organic--inorganic hybrid
 metal cluster compound ((n-C4H9)4N)2[Mo6Bri8Bra6]
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              465
_journal_page_last               470
_journal_paper_doi               10.1039/D1CE01033F
_journal_volume                  24
_journal_year                    2022
_chemical_formula_sum            'C32 H72 Br14 Mo6 N2'
_chemical_formula_weight         2179.29
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method
;
FinalCif V90 by Daniel Kratzert, Freiburg 2021,
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2021-11-03 deposited with the CCDC.	2021-12-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.481(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.0071(10)
_cell_length_b                   11.6664(9)
_cell_length_c                   19.0278(14)
_cell_measurement_reflns_used    9836
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.42
_cell_measurement_theta_min      2.35
_cell_volume                     2887.3(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1010
_diffrn_reflns_av_unetI/netI     0.0843
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            32465
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.530
_diffrn_reflns_theta_min         2.345
_exptl_absorpt_coefficient_mu    10.976
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3717
_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    2.507
_exptl_crystal_description       Chunk
_exptl_crystal_F_000             2040
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.180
_refine_diff_density_max         1.825
_refine_diff_density_min         -2.488
_refine_diff_density_rms         0.331
_refine_ls_extinction_coef       0.0018(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         6537
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0644
_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^)+(0.1105P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1660
_refine_ls_wR_factor_ref         0.1770
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5174
_reflns_number_total             6537
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01033f2.cif
_cod_data_source_block           113K
_cod_depositor_comments
'Adding full bibliography for 7244016--7244018.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7244017
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.118
_shelx_estimated_absorpt_t_max   0.243
_shelx_res_checksum              5965