Synthesis, Redox Chemistry, and Electronic Structure of the Butadiynyl and Hexatriynyl Complexes [Mo{(C≡C)nC≡CR}(L2)(η-C7H7)]z+(n= 1, 2;z= 0, 1; R = SiMe3, H; L2= 2,2′-bipyridine, Ph2PCH2CH2PPh2)
Roberts, Hannah N.; Brown, Neil J.; Edge, Ruth; Fitzgerald, Emma C.; Ta, Yien T.; Collison, David; Low, Paul J.; Whiteley, Mark W.; Organometallics 31 (2012) 6322–; doi:10.1021/om3005756

data_4079212
_publ_contact_author
; 
    Hannah Roberts
;
_publ_section_title
;
 Synthesis, Redox Chemistry, and Electronic Structure of the Butadiynyl
 and Hexatriynyl Complexes [Mo{(C\\tb C)nC\\tb CR}(L2)(\h-C7H7)]z+(n= 1,
 2;z= 0, 1; R = SiMe3, H; L2= 2,2&#x2032;-bipyridine, Ph2PCH2CH2PPh2)
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              6322
_journal_paper_doi               10.1021/om3005756
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         '2(C40 H40 Mo P2 Si), (C7)'
_chemical_formula_sum            'C87 H80 Mo2 P4 Si2'
_chemical_formula_weight         1497.45
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 99.998(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            2
_cell_length_a                   13.161(5)
_cell_length_b                   16.167(5)
_cell_length_c                   17.750(5)
_cell_measurement_reflns_used    11691
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.3434
_cell_measurement_theta_min      2.7746
_cell_volume                     3719(2)
_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 0.996
_diffrn_measured_fraction_theta_max 0.900
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_sigmaI/netI    0.0648
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25868
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.78
_exptl_absorpt_coefficient_mu    0.501
_exptl_absorpt_correction_T_max  0.9516
_exptl_absorpt_correction_T_min  0.6902
_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    1.337
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1548
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.654
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.924
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         8336
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.929
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0433P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0786
_reflns_number_gt                5896
_reflns_number_total             8336
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3005756_si_002.cif
_cod_data_source_block           Complex_3
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4079212