Synthesis and Characterization of Dimolybdenum(II) Complexes Connected by Carboxylate Linkers
Cai, Xu-Min; Höhne, Dominik; Köberl, Mathias; Cokoja, Mirza; Pöthig, Alexander; Herdtweck, Eberhardt; Haslinger, Stefan; Herrmann, Wolfgang A.; Kühn, Fritz E.; Organometallics 32 (2013) 6004–; doi:10.1021/om400518f

data_4081568
_publ_section_title
;
 Synthesis and Characterization of Dimolybdenum(II) Complexes Connected by
 Carboxylate Linkers
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              6004
_journal_paper_doi               10.1021/om400518f
_journal_volume                  32
_journal_year                    2013
_chemical_compound_source        'see text'
_chemical_formula_moiety
'C30 H30 B F4 Fe2 Mo2 N4 O4, 2(C2 H3 N), B F4'
_chemical_formula_sum            'C34 H36 B2 F8 Fe2 Mo2 N6 O4'
_chemical_formula_weight         1069.89
_chemical_name_systematic        ?
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3889(2)
_cell_length_b                   11.2996(2)
_cell_length_c                   44.7144(8)
_cell_measurement_reflns_used    5712
_cell_measurement_temperature    123
_cell_measurement_theta_max      25.1575
_cell_measurement_theta_min      2.2618
_cell_volume                     4743.79(16)
_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, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2004)'
_computing_structure_refinement
'SHELXL97 (Sheldrick, 1997), SHELXLE (Huebschle, 2011)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123
_diffrn_detector                 ' CCD plate '
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0649
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8658
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.36
_diffrn_reflns_theta_max         25.36
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    1.186
_exptl_absorpt_correction_T_max  0.897
_exptl_absorpt_correction_T_min  0.714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker, 2008b'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.090
_platon_squeeze_details
;
The unit cell contains 5 methylene chloride molecules which have been treated 
as a diffuse contribution to the overall scattering without specific atom 
positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         2.859
_refine_diff_density_min         -0.913
_refine_diff_density_rms         0.116
_refine_ls_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         8658
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0537P)^2^+8.8786P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1114
_refine_ls_wR_factor_ref         0.1182
_reflns_number_gt                6891
_reflns_number_total             8658
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om400518f_si_002.cif
_cod_data_source_block           caixu3_0m-sr
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_database_code               4081568