Molybdenum 17- and 18-Electron Bis- and Tris(Butadiene) Complexes: Electronic Structures, Spectroscopic Properties, and Oxidative Ligand Substitution Reactions
Gerald C. Stephan; Christian Näther; Gerhard Peters; Felix Tuczek; Inorganic Chemistry 52 (2013) 5931–5942; doi:10.1021/ic400145f

data_4334873
_publ_section_title
;
 Molybdenum 17- and 18-Electron Bis- and Tris(Butadiene) Complexes:
 Electronic Structures, Spectroscopic Properties, and Oxidative Ligand
 Substitution Reactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5931
_journal_page_last               5942
_journal_paper_doi               10.1021/ic400145f
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C52 H48 B F6 Mo P4'
_chemical_formula_weight         1017.53
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.678(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.8666(5)
_cell_length_b                   22.5280(16)
_cell_length_c                   21.1750(11)
_cell_measurement_temperature    170(2)
_cell_volume                     4701.5(5)
_computing_cell_refinement       'IPDS-1 program package'
_computing_data_collection       'IPDS-1 program package'
_computing_data_reduction        'IPDS-1 program package'
_computing_molecular_graphics    'XP in SHELXTL-PC'
_computing_publication_material  SHELXTL-PC
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'STOE IPDS-1'
_diffrn_measurement_method       'Phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0329
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            23978
_diffrn_reflns_theta_full        28.06
_diffrn_reflns_theta_max         28.06
_diffrn_reflns_theta_min         2.41
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.475
_exptl_absorpt_correction_T_max  0.9067
_exptl_absorpt_correction_T_min  0.7242
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'STOE X-Shape and X-Red)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_description       block
_exptl_crystal_F_000             2084
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.024(18)
_refine_ls_extinction_coef       0.0048(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         11122
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0324
_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^)+(0.0534P)^2^+2.6107P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0808
_refine_ls_wR_factor_ref         0.0817
_reflns_number_gt                10612
_reflns_number_total             11122
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400145f_si_004.cif
_cod_data_source_block           felix52
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4334873