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_4079213
_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         'C26 H15 Mo N2 Si'
_chemical_formula_sum            'C26 H15 Mo N2 Si'
_chemical_formula_weight         479.43
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.940(5)
_cell_angle_beta                 96.832(5)
_cell_angle_gamma                94.964(5)
_cell_formula_units_Z            2
_cell_length_a                   8.492(5)
_cell_length_b                   10.802(5)
_cell_length_c                   14.077(5)
_cell_measurement_reflns_used    2648
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      28.4947
_cell_measurement_theta_min      2.6691
_cell_volume                     1194.0(10)
_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      220(2)
_diffrn_detector_area_resol_mean 8.3367
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.986
_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  0.0630
_diffrn_reflns_av_sigmaI/netI    0.1272
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6816
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         3.77
_exptl_absorpt_coefficient_mu    0.613
_exptl_absorpt_correction_T_max  0.9939
_exptl_absorpt_correction_T_min  0.7493
_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            brown
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             482
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.910
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         4147
_refine_ls_number_restraints     241
_refine_ls_restrained_S_all      0.891
_refine_ls_R_factor_all          0.1013
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1137
_reflns_number_gt                2573
_reflns_number_total             4147
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3005756_si_002.cif
_cod_data_source_block           Complex_5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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-1
_cod_database_code               4079213