Molecular and Electronic Structures of Six-Coordinate "Low-Valent" [M(Mebpy)3]0 (M = Ti, V, Cr, Mo) and [M(tpy)2]0 (M = Ti, V, Cr), and Seven-Coordinate [MoF(Mebpy)3](PF6) and [MX(tpy)2](PF6) (M = Mo, X = Cl and M = W, X = F)
Mei Wang; Thomas Weyhermüller; Jason England; Karl Wieghardt; Inorganic Chemistry 52 (2013) 12763–12776; doi:10.1021/ic402037e

data_4336633
_publ_section_title
;
 Molecular and Electronic Structures of Six-Coordinate "Low-Valent"
 [M(Mebpy)3]0 (M = Ti, V, Cr, Mo) and [M(tpy)2]0 (M = Ti, V, Cr), and
 Seven-Coordinate [MoF(Mebpy)3](PF6) and [MX(tpy)2](PF6) (M = Mo, X = Cl
 and M = W, X = F)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12763
_journal_page_last               12776
_journal_paper_doi               10.1021/ic402037e
_journal_volume                  52
_journal_year                    2013
_chemical_compound_source        dichloromethane
_chemical_formula_moiety         'C30 H22 F N6 W, F6 P, C H2 Cl2'
_chemical_formula_sum            'C31 H24 Cl2 F7 N6 P W'
_chemical_formula_weight         899.28
_chemical_name_systematic
; 
 ? 
;
_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
_audit_block_code                WGT-SW-018-01
_audit_creation_date             2011-05-24
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.264(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.3478(13)
_cell_length_b                   18.0554(9)
_cell_length_c                   11.7524(10)
_cell_measurement_reflns_used    70560
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.0993
_cell_measurement_theta_min      2.657
_cell_volume                     3074.4(4)
_computing_cell_refinement       'DENZO (Bruker AXS, 2006)'
_computing_data_collection       'DATCOL (Bruker AXS, 2006)'
_computing_data_reduction        'DENZO (Bruker AXS, 2006)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 18.02
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker AXS Enraf-Nonius KappaCCD'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0621
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            65675
_diffrn_reflns_theta_full        33.08
_diffrn_reflns_theta_max         33.08
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    4.061
_exptl_absorpt_correction_T_max  0.89526
_exptl_absorpt_correction_T_min  0.53623
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.943
_exptl_crystal_description       plate
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.960
_refine_diff_density_min         -2.807
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         11646
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0000P)^2^+11.2114P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0626
_refine_ls_wR_factor_ref         0.0690
_reflns_number_gt                9054
_reflns_number_total             11646
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402037e_si_002_8.cif
_cod_data_source_block           12
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4336633