Bis[(±)-<i>trans</i>-2-aminocyclohexylammonium] tetrathiomolybdate(VI) and <i>trans</i>-cyclohexane-1,4-diammonium tetrathiomolybdate(VI)
Srinivasan, Bikshandarkoil R.; Näther, Christian; Bensch, Wolfgang; Acta Crystallographica Section C 62 (2006) m98–m101; doi:10.1107/S0108270106001685

data_2014301
_publ_section_title
;
 Bis[(+-)-<i>trans</i>-2-aminocyclohexylammonium]
 tetrathiomolybdate(VI) and <i>trans</i>-cyclohexane-1,4-diammonium
 tetrathiomolybdate(VI)
;
_journal_coeditor_code           AV1276
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m98
_journal_page_last               m101
_journal_paper_doi               10.1107/S0108270106001685
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '(C6 H15 N2)2 [Mo S4]'
_chemical_formula_moiety         '2C6 H15 N2 +, Mo S4 2-'
_chemical_formula_sum            'C12 H30 Mo N4 S4'
_chemical_formula_weight         454.58
_chemical_name_common
;
((+-)trans-1,2cnH)~2~ tetrathiomolybdate(VI)
;
_chemical_name_systematic
;
Bis[(+-)trans-2-aminocyclohexylammonium] tetrathiomolybdate(VI)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.736(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.279(3)
_cell_length_b                   9.4502(11)
_cell_length_c                   11.3308(16)
_cell_measurement_reflns_used    74
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19
_cell_measurement_theta_min      10
_cell_volume                     1966.2(5)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1998)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1998)'
_computing_molecular_graphics    'XP in SHELXTL (Bruker, 1998)'
_computing_publication_material  'CIFTAB in SHELXTL'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Stoe AED-II four-circle diffractometer'
_diffrn_measurement_method       '\w--\q scan'
_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  0.0166
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       2
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3593
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         2.22
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  2h
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    1.091
_exptl_absorpt_correction_T_max  0.909
_exptl_absorpt_correction_T_min  0.889
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-Shape; Stoe & Cie, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.318
_refine_ls_extinction_coef       0.00056(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         2863
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0244
_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^)+(0.0257P)^2^+1.4007P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0565
_refine_ls_wR_factor_ref         0.0605
_reflns_number_gt                2357
_reflns_number_total             2863
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            av1276.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               2014301
_cod_database_fobs_code          2014301