Jahn-Teller distortion of the open-shell 23-electron chalcogenide rhenium cluster cores in crystals of the series, {[Re~6~Q~8~]^3+^(X^-^)~6~}^3-^ (Q = S, Se; X = Cl, CN)
Baudron, Stéphane A.; Deluzet, André; Boubekeur, Kamal; Batail, Patrick; Chemical Communications  (2002) 2124–2125; doi:10.1039/b205241e

data_7114038
_publ_section_title
;
 Jahn-Teller distortion of the open-shell 23-electron chalcogenide
 rhenium cluster cores in crystals of the series, 
{[Re~6~Q~8~]^3+^(X^-^)~6~}^3-^ (Q = S, Se; X = Cl, CN)
;
_journal_issue                   18
_journal_name_full               'Chemical Communications'
_journal_page_first              2124
_journal_page_last               2125
_journal_paper_doi               10.1039/b205241e
_journal_year                    2002
_chemical_formula_sum            'C80 H69 N7 O3 P3 Re6 Se8'
_chemical_formula_weight         3018.21
_chemical_name_common            '(PPh4)3 (RE6Se8(CN)6) CH3CN (H2O)3'
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                74.976(8)
_cell_angle_beta                 89.776(8)
_cell_angle_gamma                62.578(8)
_cell_formula_units_Z            2
_cell_length_a                   13.4983(9)
_cell_length_b                   14.1705(10)
_cell_length_c                   25.9583(19)
_cell_measurement_reflns_used    7995
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      52.1
_cell_measurement_theta_min      3.3
_cell_volume                     4217.9(7)
_computing_cell_refinement       'SELECT, CELL [STOE-IPDS]'
_computing_data_collection       'EXPOSE [STOE-IPDS]'
_computing_data_reduction        'INTEGRATE [STOE-IPDS]'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  STOE-IPDS
_diffrn_measurement_method       'Oscillation, PHi. incr. == 0.9'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_sigmaI/netI    0.0497
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            41780
_diffrn_reflns_theta_full        25.88
_diffrn_reflns_theta_max         25.88
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    12.134
_exptl_absorpt_correction_T_max  0.2469
_exptl_absorpt_correction_T_min  0.0531
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'FACEIT, STOE-IPDS'
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    2.376
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2778
_exptl_crystal_size_max          0.4620
_exptl_crystal_size_mid          0.3850
_exptl_crystal_size_min          0.1386
_refine_diff_density_max         1.985
_refine_diff_density_min         -1.321
_refine_diff_density_rms         0.192
_refine_ls_extinction_coef       0.000068(10)
_refine_ls_extinction_expression Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.903
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     948
_refine_ls_number_reflns         15278
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.903
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0244
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w==1/[\s^2^(Fo^2^)+(0.0230P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0504
_refine_ls_wR_factor_ref         0.0554
_reflns_number_gt                11832
_reflns_number_total             15278
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b205241e.txt
_cod_data_source_block           sb280150_abmerge
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        4217.9(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7114038