Coordination compounds containing bis-dithiolene-chelated molybdenum(IV) and oxalate: comparison of terminal with bridging oxalate
Gapinska, Agata; Lough, Alan J.; Fekl, Ulrich; Acta Crystallographica Section E 73 (2017) 1202–1207; doi:10.1107/S205698901701026X

data_2242109
_publ_section_title
;
 Coordination compounds containing bis-dithiolene-chelated molybdenum(IV)
 and oxalate: comparison of terminal with bridging oxalate
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1202
_journal_page_last               1207
_journal_paper_doi               10.1107/S205698901701026X
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '(C16 H36 N) [Mo2 (C4 F6 S2)4 (C2 O4)]'
_chemical_formula_moiety         '2(C16 H36 N +), C18 F24 Mo2 O4 S8 2-'
_chemical_formula_sum            'C50 H72 F24 Mo2 N2 O4 S8'
_chemical_formula_weight         1669.45
_chemical_name_systematic
;Bis(tetra-<i>n</i>-butylammonium)
\m-oxalato-bis[bis(1,1,1,4,4,4-hexafluorobut-2-ene-2,3-dithiolato)molybdate(IV)]
;
_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
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_cell_angle_alpha                90
_cell_angle_beta                 103.159(5)
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_cell_formula_units_Z            2
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_cell_length_b                   19.4940(19)
_cell_length_c                   14.4056(14)
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_cell_measurement_temperature    150(2)
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_computing_cell_refinement
;
DENZO-SMN (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
COLLECT (Nonius, 2002)
;
_computing_data_reduction
;
DENZO-SMN (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics
;
ORTEP-3 (Farrugia, 2012) and PLATON (Spek, 2009)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR92 (Altomare <i>et al.</i>,  1994)
;
_diffrn_ambient_temperature      150(2)
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_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scan and \w scans with \k offsets'
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_diffrn_reflns_av_R_equivalents  0.0660
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_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.827
_diffrn_reflns_theta_min         2.768
_exptl_absorpt_coefficient_mu    0.631
_exptl_absorpt_correction_T_max  0.931
_exptl_absorpt_correction_T_min  0.720
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SORTAV; Blessing, 1995)
;
_exptl_crystal_colour            green
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_exptl_crystal_description       plate
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_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.060
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_refine_diff_density_min         -0.654
_refine_ls_extinction_method     none
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_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.1220
_refine_ls_R_factor_gt           0.0652
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0589P)^2^+6.7410P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_ref         0.1640
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_reflns_threshold_expression     'I > 2\s(I)'
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_shelx_estimated_absorpt_t_min   0.895
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_shelx_fab_checksum              2454
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