Synthesis and characterization of dimeric and square-shaped dicarboxylate-bridged dimolybdenum(II) coordination compounds
Dominik Hohne; Eberhardt Herdtweck; Alexander Pothig; Fritz E. Kuhn; Inorganica Chimica Acta 424 (2015) 210–215; doi:

data_1518861
_publ_section_title
;
 Synthesis and characterization of dimeric and square-shaped
 dicarboxylate-bridged dimolybdenum(II) coordination compounds
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              210
_journal_page_last               215
_journal_volume                  424
_journal_year                    2015
_chemical_formula_moiety         'C56 H56 Mo8 N16 O16 S4, 8(B F4), 8(C2 H3 N)'
_chemical_formula_sum            'C72 H80 B8 F32 Mo8 N24 O16 S4'
_chemical_formula_weight         3127.88
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                70.855(3)
_cell_angle_beta                 87.566(3)
_cell_angle_gamma                80.438(3)
_cell_formula_units_Z            1
_cell_length_a                   12.4639(7)
_cell_length_b                   17.9126(11)
_cell_length_c                   20.0691(12)
_cell_measurement_reflns_used    9763
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      25.51
_cell_measurement_theta_min      1.22
_cell_volume                     4173.7(4)
_computing_cell_refinement       'SAINT (Bruker, 2008b)'
_computing_data_collection       'APEX II Control Software (Bruker, 2008a)'
_computing_data_reduction        'SAINT (Bruker, 2008b)'
_computing_molecular_graphics    'PLATON (Spek, 2010)'
_computing_publication_material  'PLATON (Spek, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1998)'
_computing_structure_solution    'SIR92 (Altomare, 1994)'
_diffrn_ambient_temperature      123(1)
_diffrn_detector                 ' CCD plate '
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       ' \k-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker APEX-II CCD '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode FR591'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            83914
_diffrn_reflns_theta_full        25.51
_diffrn_reflns_theta_max         25.51
_diffrn_reflns_theta_min         1.22
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.712
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6312
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker, 2008b'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.214
_refine_diff_density_min         -0.979
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     789
_refine_ls_number_reflns         15404
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0604
_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^)+(0.0805P)^2^+12.0324P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.1560
_refine_ls_wR_factor_ref         0.1637
_reflns_number_gt                12357
_reflns_number_total             15404
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ICA-2015-424-210-215-2.cif
_cod_data_source_block           4
_cod_database_code               1518861