Synthesis of chromium(0) and molybdenum(0) bis (eta(6)-arene) derivatives and their monoelectronic oxidation to [M(eta(6)-arene)(2)](+) cations.
Calucci, Lucia; Cloke, F Geoffrey N; Englert, Ulli; Hitchcock, Peter B.; Pampaloni, Guido; Pinzino, Calogero; Puccini, Filippo; Volpe, Manuel; Dalton transactions (Cambridge, England : 2003)  (2006) 4228–4234; doi:10.1039/b602783k

data_7007282
_publ_section_title
;
 Synthesis of chromium(0) and molybdenum(0) bis (eta(6)-arene)
 derivatives and their monoelectronic oxidation to
 [M(eta(6)-arene)(2)](+) cations.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4228
_journal_page_last               4234
_journal_paper_doi               10.1039/b602783k
_journal_year                    2006
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C30 H48 Mo, C15 H15 O10, 2(C4 H8 O)'
_chemical_formula_sum            'C53 H79 Mo O12'
_chemical_formula_weight         1004.1
_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
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2004-07-21T11:34:06-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                75.820(2)
_cell_angle_beta                 84.673(2)
_cell_angle_gamma                76.999(2)
_cell_formula_units_Z            2
_cell_length_a                   11.6201(5)
_cell_length_b                   12.7552(5)
_cell_length_c                   18.5897(7)
_cell_measurement_reflns_used    37528
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     2600.80(18)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.379078E-1
_diffrn_orient_matrix_UB_12      -0.254529E-1
_diffrn_orient_matrix_UB_13      0.498718E-1
_diffrn_orient_matrix_UB_21      -0.788037E-1
_diffrn_orient_matrix_UB_22      0.425078E-1
_diffrn_orient_matrix_UB_23      -0.189922E-1
_diffrn_orient_matrix_UB_31      -0.128915E-1
_diffrn_orient_matrix_UB_32      -0.662135E-1
_diffrn_orient_matrix_UB_33      -0.15345E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33339
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.24
_diffrn_reflns_theta_min         3.73
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.311
_exptl_absorpt_correction_T_max  0.9846
_exptl_absorpt_correction_T_min  0.8901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1070
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.706
_refine_diff_density_min         -1.133
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         9150
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.094
_refine_ls_R_factor_gt           0.0643
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0811P)^2^+7.8721P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1591
_refine_ls_wR_factor_ref         0.1774
_reflns_number_gt                6562
_reflns_number_total             9150
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b602783k.txt
_cod_data_source_block           jul1904
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7007282