Crystal structure of bis(tetrabutylammonium) oxopentathiocyanatomolybdate(V) — ethanol (1:0.5), [(C4H9)4N]2[MoO(NCS)5] · 0.5C2H5OH
Jiake Chen; Pingfan Wu; Zicheng Xiao; Jian Hao; Zeitschrift für Kristallographie - New Crystal Structures 225 (2010) 577–; doi:

data_8102776
_publ_section_title
;
 Crystal structure of bis(tetrabutylammonium)
 oxopentathiocyanatomolybdate(V) --- ethanol (1:0.5),
 [(C4H9)4N]2[MoO(NCS)5] &#x00B7; 0.5C2H5OH
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              577
_journal_volume                  225
_journal_year                    2010
_chemical_formula_moiety         '2(C16 H36 N), 0.5(C2 H6 O), (C5 Mo N5 O S5)'
_chemical_formula_sum            'C38 H75 Mo N7 O1.5 S5'
_chemical_formula_weight         910.29
_chemical_name_systematic
;
Bis(tetrabutylammonium) Oxopentathiocyanatomolybdate(V)
;
_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                111.27(3)
_cell_angle_beta                 112.36(3)
_cell_angle_gamma                92.36(3)
_cell_formula_units_Z            4
_cell_length_a                   16.282(3)
_cell_length_b                   17.261(4)
_cell_length_c                   21.234(4)
_cell_measurement_reflns_used    64400
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.395
_cell_volume                     5031(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD (Nonius B. V., 1998)'
_computing_data_reduction
'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.76
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_diffrn_measurement_method       CCD
_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  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0416
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            37529
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.41
_exptl_absorpt_coefficient_mu    0.503
_exptl_absorpt_correction_T_max  0.844
_exptl_absorpt_correction_T_min  0.771
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.949
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     979
_refine_ls_number_reflns         19666
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0451P)^2^+2.3695P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0959
_refine_ls_wR_factor_ref         0.1072
_reflns_number_gt                13727
_reflns_number_total             19666
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-3075.cff
_cod_data_source_block           '[BuN4]2[MoO(NCS)5]'
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C38 H75 Mo N7 O1.50 S5'
_cod_database_code               8102776