Orbital Symmetry Control of Electronic Coupling in a Symmetrical, All-Carbon-Bridged “Mixed Valence” Compound: Synthesis, Spectroscopy, and Electronic Structure of [{Mo(dppe)(η-C7H7)}2(μ-C4)]n+(n= 0, 1, or 2)
Fitzgerald, Emma C.; Brown, Neil J.; Edge, Ruth; Helliwell, Madeleine; Roberts, Hannah N.; Tuna, Floriana; Beeby, Andrew; Collison, David; Low, Paul J.; Whiteley, Mark W.; Organometallics 31 (2012) 157–; doi:10.1021/om200712m

data_4067815
_publ_contact_author
; 
    Hannah Roberts
;
_publ_section_title
;
 Orbital Symmetry Control of Electronic Coupling in a Symmetrical,
 All-Carbon-Bridged &#x201C;Mixed Valence&#x201D; Compound: Synthesis,
 Spectroscopy, and Electronic Structure of
 [{Mo(dppe)(\h-C7H7)}2(\m-C4)]n+(n= 0, 1, or 2)
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              157
_journal_paper_doi               10.1021/om200712m
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C73 H67 F12 Mo2 N1.5 O0.25 P6'
_chemical_formula_weight         1574.98
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 97.174(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   58.826(3)
_cell_length_b                   11.7374(9)
_cell_length_c                   19.7396(11)
_cell_measurement_reflns_used    4186
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.4181
_cell_measurement_theta_min      2.6134
_cell_volume                     13522.8(15)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3367
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford Diffraction XCalibur 2'
_diffrn_measurement_method       'phi and omega'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0886
_diffrn_reflns_av_sigmaI/netI    0.1977
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -70
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24834
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    0.591
_exptl_absorpt_correction_T_max  0.8909
_exptl_absorpt_correction_T_min  0.7978
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6396
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.185
_refine_diff_density_min         -0.780
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.877
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     961
_refine_ls_number_reflns         11910
_refine_ls_number_restraints     714
_refine_ls_restrained_S_all      0.870
_refine_ls_R_factor_all          0.1306
_refine_ls_R_factor_gt           0.0605
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0581P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1260
_refine_ls_wR_factor_ref         0.1403
_reflns_number_gt                6051
_reflns_number_total             11910
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200712m_si_002.cif
_cod_data_source_block           omww46C
_cod_original_cell_volume        13522.9(15)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C73 H67 F12 Mo2 N1.50 O0.25 P6'
_cod_database_code               4067815