Metallacumulenylidene Complexes in the Cycloheptatrienyl Molybdenum Series [Mo{(C)nCR2}L2(η-C7H7)]+(n= 0−2; L2= P-Donor Ligand). X-ray Crystal Structures of [Mo{CC(H)Ph}{P(OMe)3}2(η-C7H7)][BF4] and [Mo(CCCPh2)(dppe)(η-C7H7)][PF6] and DFT Investigation of Cumulenylidene Ligand Orientations
Grime, Richard W.; Helliwell, Madeleine; Hussain, Zaffar I.; Lancashire, Hannah N.; Mason, Christopher R.; McDouall, Joseph J. W.; Mydlowski, Christopher M.; Whiteley, Mark W.; Organometallics 27 (2008) 857–; doi:10.1021/om700920t

data_4070518
_publ_contact_author
;
Madeleine Helliwell 

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_publ_section_title
;
 Metallacumulenylidene Complexes in the Cycloheptatrienyl Molybdenum
 Series [Mo{(C)n&#xE5FB;CR2}L2(\h-C7H7)]+(n= 0&#x2212;2; L2= P-Donor
 Ligand). X-ray Crystal Structures of
 [Mo{C&#xE5FB;C(H)Ph}{P(OMe)3}2(\h-C7H7)][BF4] and
 [Mo(C&#xE5FB;C&#xE5FB;CPh2)(dppe)(\h-C7H7)][PF6] and DFT Investigation of
 Cumulenylidene Ligand Orientations
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_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              857
_journal_paper_doi               10.1021/om700920t
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C22 H35 B F4 Mo O7 P2'
_chemical_formula_weight         656.19
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.439(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5384(14)
_cell_length_b                   13.0298(17)
_cell_length_c                   20.266(3)
_cell_measurement_reflns_used    4656
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.32
_cell_measurement_theta_min      2.24
_cell_volume                     2777.8(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0499
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15368
_diffrn_reflns_theta_full        26.46
_diffrn_reflns_theta_max         26.46
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    0.653
_exptl_absorpt_correction_T_max  0.9376
_exptl_absorpt_correction_T_min  0.8282
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.636
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         5686
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0352P)^2^+0.5326P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0780
_reflns_number_gt                4573
_reflns_number_total             5686
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            compd8cif.cif
_cod_data_source_block           h:\s2065\work\s2065abs
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2777.8(6)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4070518