Rational Synthesis and Characterization of Dimolybdenum(II) Compounds Bearing Ferrocenyl-Containing Ligands toward Modulation of Electronic Coupling.
Cai, Xu-Min; Riener, Korbinian; Herdtweck, Eberhardt; Pöthig, Alexander; Kühn, Fritz E; Inorganic chemistry  (2015) 150317135657008–; doi:10.1021/ic502913w

data_4343011
_publ_section_title
;
 Rational Synthesis and Characterization of Dimolybdenum(II) Compounds
 Bearing Ferrocenyl-Containing Ligands toward Modulation of Electronic
 Coupling.
;
_journal_name_full               'Inorganic chemistry'
_journal_page_first              150317135657008
_journal_paper_doi               10.1021/ic502913w
_journal_year                    2015
_chemical_formula_moiety         'C72 H62 Fe2 Mo2 O4 P4, 2(C2 H3 N), 2(B F4)'
_chemical_formula_sum            'C76 H68 B2 F8 Fe2 Mo2 N2 O4 P4'
_chemical_formula_weight         1674.40
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 107.2383(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.0024(5)
_cell_length_b                   12.7260(4)
_cell_length_c                   23.2277(8)
_cell_measurement_reflns_used    9717
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      25.39
_cell_measurement_theta_min      1.84
_cell_volume                     3953.1(2)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0136
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            80760
_diffrn_reflns_theta_full        25.39
_diffrn_reflns_theta_max         25.39
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.816
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6602
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker, 2008b'
_exptl_crystal_colour            'red brown'
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
;
_refine_diff_density_max         2.105
_refine_diff_density_min         -0.933
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         7243
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0438
_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^)+(0.0417P)^2^+18.0338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.1125
_refine_ls_wR_factor_ref         0.1141
_reflns_number_gt                6663
_reflns_number_total             7243
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic502913w_si_002.cif
_cod_data_source_block           Compound_2b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4343011