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_1518860
_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         'C36 H42 Br4 Mo4 N14 O4, 6(B F4)'
_chemical_formula_sum            'C36 H42 B6 Br4 F24 Mo4 N14 O4'
_chemical_formula_weight         1959.06
_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                93.187(5)
_cell_angle_beta                 103.746(5)
_cell_angle_gamma                118.080(4)
_cell_formula_units_Z            1
_cell_length_a                   11.3474(11)
_cell_length_b                   11.7560(11)
_cell_length_c                   17.0657(16)
_cell_measurement_reflns_used    9647
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      25.39
_cell_measurement_theta_min      1.25
_cell_volume                     1913.5(3)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0541
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            57939
_diffrn_reflns_theta_full        25.39
_diffrn_reflns_theta_max         25.39
_diffrn_reflns_theta_min         1.25
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.828
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4440
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker, 2008b'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_density_method    none
_exptl_crystal_description       fragment
_exptl_crystal_F_000             942
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.932
_refine_diff_density_min         -0.832
_refine_diff_density_rms         0.117
_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     422
_refine_ls_number_reflns         7000
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0552P)^2^+1.9991P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.0948
_reflns_number_gt                6046
_reflns_number_total             7000
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ICA-2015-424-210-215-1.cif
_cod_data_source_block           2
_cod_database_code               1518860