Proton motion inside [(DMF)<sub>2</sub>H]<sub>2</sub>[W<sub>6</sub>Cl<sub>14</sub>]: structural, Raman and luminescence studies.
Kolesov, Boris A.; Chupina, Anastasia V.; Berezin, Alexey S.; Kompankov, Nikolay B.; Abramov, Pavel A.; Sokolov, Maxim N.; Physical chemistry chemical physics : PCCP 22 (2020) 25344–25352; doi:10.1039/d0cp04152a

data_7241380
_publ_section_title
;
 Proton motion inside
 [(DMF)<sub>2</sub>H]<sub>2</sub>[W<sub>6</sub>Cl<sub>14</sub>]:
 structural, Raman and luminescence studies.
;
_journal_issue                   43
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              25344
_journal_page_last               25352
_journal_paper_doi               10.1039/d0cp04152a
_journal_volume                  22
_journal_year                    2020
_chemical_formula_sum            'C12 H30 Cl14 N4 O4 W6'
_chemical_formula_weight         1893.80
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2020-07-30 deposited with the CCDC.	2020-10-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.9480(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.6059(3)
_cell_length_b                   10.3846(3)
_cell_length_c                   17.1139(5)
_cell_measurement_reflns_used    9376
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      30.4766
_cell_measurement_theta_min      2.7551
_cell_volume                     1871.05(9)
_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      85(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-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  0.0406
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            49924
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         30.512
_diffrn_reflns_theta_min         2.755
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    19.396
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5104
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.361
_exptl_crystal_description       prism
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.116
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.559
_refine_diff_density_min         -1.641
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         5693
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0202
_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^)+(0.0064P)^2^+6.1393P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0411
_refine_ls_wR_factor_ref         0.0429
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5204
_reflns_number_total             5693
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            d0cp04152a2.cif
_cod_data_source_block           85
_cod_depositor_comments
'Adding full bibliography for 7241380--7241382.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7241380
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.212
_shelx_estimated_absorpt_t_max   0.444
_shelx_res_checksum              55002