Iron‒Molybdenum Charge-Transfer Hybrids Containing Organometallic and Inorganic Fragments Bridged by Aryldiazenido Ligands in a μ-η6:η1 Coordination Mode: Syntheses, Characterization, X-ray Structures, Electrochemistry, and Theoretical Investigation
Manzur, Carolina; Millán, Lorena; Fuentealba, Mauricio; Hamon, Jean-René; Toupet, Loïc; Kahlal, Samia; Saillard, Jean-Yves; Carrillo, David; Inorganic Chemistry 46 (2007) 1123–1134; doi:10.1021/ic0613098

data_4306953
_publ_section_title
;
 Iron--Molybdenum Charge-Transfer Hybrids Containing Organometallic
 and Inorganic Fragments Bridged by Aryldiazenido Ligands in a
 \m-\h6:\h1 Coordination Mode: Syntheses, Characterization, X-ray
 Structures, Electrochemistry, and Theoretical Investigation
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   4
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1123
_journal_page_last               1134
_journal_paper_doi               10.1021/ic0613098
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C27 H42 F6 Fe Mo N5 O P S6'
_chemical_formula_weight         941.77
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.994(3)
_cell_angle_beta                 93.952(3)
_cell_angle_gamma                107.908(3)
_cell_formula_units_Z            4
_cell_length_a                   10.0854(3)
_cell_length_b                   16.2396(7)
_cell_length_c                   25.2360(9)
_cell_measurement_temperature    120(1)
_cell_volume                     3911.9(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Nonius (1999)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'PLATON_(Spek, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97_(Altomare & al., 1998)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 19.24
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  Nonius_KappaCCD
_diffrn_measurement_method       'Area detector scans (see text)'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0797
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            17367
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    1.111
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.051
_refine_diff_density_min         -0.672
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         17367
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.1732
_refine_ls_R_factor_gt           0.0776
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0216P)^2^+35.5859P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1578
_refine_ls_wR_factor_ref         0.1942
_reflns_number_gt                10662
_reflns_number_total             17367
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0613098si20060714_035705.cif
_cod_data_source_block           jrhmo120k
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        3911.9(2)
_cod_database_code               4306953