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_2242108
_publ_section_title
;
 Coordination compounds containing bis-dithiolene-chelated molybdenum(IV)
 and oxalate: comparison of terminal with bridging oxalate
;
_journal_coeditor_code           ZL2708
_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)2 [Mo (C4 F6 S2)2 (C2 O4)], C2 H2 O4, C H Cl3'
_chemical_formula_moiety
'2(C16 H36 N +), C10 F12 Mo O4 S4 2-, C2 H2 O4, C H Cl3'
_chemical_formula_sum            'C45 H75 Cl3 F12 Mo N2 O8 S4'
_chemical_formula_weight         1330.60
_chemical_name_systematic
;Bis(tetra-<i>n</i>-butylammonium)
bis(1,1,1,4,4,4-hexafluorobut-2-ene-2,3-dithiolato)oxalatomolybdate(IV)--chloroform--oxalic acid (1/1/1),
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3879(2)
_cell_length_b                   17.8733(5)
_cell_length_c                   22.2895(6)
_cell_measurement_reflns_used    31375
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     6130.3(3)
_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)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offsets'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0651
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            40314
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.636
_exptl_absorpt_coefficient_mu    0.564
_exptl_absorpt_correction_T_max  0.869
_exptl_absorpt_correction_T_min  0.759
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SORTAV (Blessing, 1995)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_description       Block
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.613
_refine_diff_density_min         -0.659
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 3456 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.036(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     816
_refine_ls_number_reflns         13841
_refine_ls_number_restraints     465
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0480
_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^)+(0.0407P)^2^+1.6697P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0898
_refine_ls_wR_factor_ref         0.1050
_reflns_number_gt                9858
_reflns_number_total             13841
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl2708sup1.cif
_cod_data_source_block           k10131
_cod_database_code               2242108
_cod_database_fobs_code          2242108
_shelx_estimated_absorpt_t_min   0.920
_shelx_estimated_absorpt_t_max   0.946
_shelx_hkl_checksum              91306
_shelx_res_checksum              56594