Crystal structure of bis(tetrabutylammonium) tetradecabromohexamolybdate, [(C~4~H~9~)~4~N]~2~[Mo~6~Br~14~], at 100 K and 293 K
K. Kirakci; S. Cordier; T. Roisnel; S. Golhen; C. Perrin; Zeitschrift für Kristallographie - New Crystal Structures 220 (2005) 116–118; doi:

data_8101711
_publ_section_title
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Crystal structure of bis(tetrabutylammonium) tetradecabromohexamolybdate, 
[(C~4~H~9~)~4~N]~2~[Mo~6~Br~14~], at 100 K and 293 K 
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_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              116
_journal_page_last               118
_journal_volume                  220
_journal_year                    2005
_chemical_formula_structural     'C32 H72 Br14 Mo6 N2'
_chemical_formula_sum            'C32 H72 Br14 Mo6 N2'
_chemical_formula_weight         2179.29
_chemical_name_systematic
;
bis(tetrabutylammonium) tetradecabromohexamolybdate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 90.8430(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.2110(2)
_cell_length_b                   11.8530(2)
_cell_length_c                   18.9280(4)
_cell_measurement_reflns_used    38194
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.91
_cell_volume                     2963.61(9)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Giacovazzo, 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0786
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            41381
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    10.691
_exptl_absorpt_correction_T_max  0.2512
_exptl_absorpt_correction_T_min  0.1820
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
[Sheldrick, G.M. (2002). SADABS version 2.03.Bruker AXS Inc., Madison,
Wisconsin, USA]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.442
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1956
_exptl_crystal_size_max          0.165
_exptl_crystal_size_mid          0.149
_exptl_crystal_size_min          0.133
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         6797
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0972
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0112P)^2^+8.9646P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0574
_refine_ls_wR_factor_ref         0.0719
_reflns_number_gt                3956
_reflns_number_total             6797
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-1446.cff
_cod_data_source_block           tbabr293
_cod_depositor_comments
;
The following automatic conversions were performed:
'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 
;
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               8101711