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_4336626
_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_formula_sum            'C36 H36 N6 Ti'
_chemical_formula_weight         600.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_block_code                WGT-WM-016-02
_audit_creation_date             2013-04-24
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 109.727(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.763(2)
_cell_length_b                   18.532(4)
_cell_length_c                   14.613(3)
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.0205
_cell_measurement_theta_min      2.2237
_cell_volume                     2998.6(10)
_computing_cell_refinement       'SAINT software (Bruker AXS, 2004)'
_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT software (Bruker AXS, 2004)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (G. M. Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 66.67
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker-AXS Kappa Mach3 APEX-II'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  'Incoatec Helios mirrors'
_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  0.0692
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            36590
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.069
_diffrn_reflns_theta_min         1.844
_exptl_absorpt_coefficient_mu    0.322
_exptl_absorpt_correction_T_max  0.98003
_exptl_absorpt_correction_T_min  0.91014
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_description       needle
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.311
_refine_diff_density_min         -1.022
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         5236
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0958
_refine_ls_R_factor_gt           0.0857
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1033P)^2^+11.3205P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2419
_refine_ls_wR_factor_ref         0.2507
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4399
_reflns_number_total             5236
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic402037e_si_002_1.cif
_cod_data_source_block           1
_cod_database_code               4336626
_shelxl_version_number           2013-2