Oligomerization of Phenylacetylene to Coordinated 2,3,6-Triphenylfulvene in Molybdenum Tetracyclone Complexes
Adams, Harry; Brown, Patrick; Cook, Elizabeth S.; Hanson, Robert J.; Morris, Michael J.; Organometallics 31 (2012) 7622–; doi:10.1021/om3008844

data_4079614
_publ_section_title
;
 Oligomerization of Phenylacetylene to Coordinated 2,3,6-Triphenylfulvene
 in Molybdenum Tetracyclone Complexes
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              7622
_journal_paper_doi               10.1021/om3008844
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C54 H38 Mo O2'
_chemical_formula_weight         814.78
_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                90.00
_cell_angle_beta                 96.953(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.304(2)
_cell_length_b                   12.9649(17)
_cell_length_c                   31.376(4)
_cell_measurement_reflns_used    3439
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      42.277
_cell_measurement_theta_min      4.462
_cell_volume                     7794.9(16)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker smart 1000'
_diffrn_measurement_method       '\w 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  0.1664
_diffrn_reflns_av_sigmaI/netI    0.2316
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            52251
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.62
_diffrn_reflns_theta_min         1.31
_exptl_absorpt_coefficient_mu    0.381
_exptl_absorpt_correction_T_max  0.9312
_exptl_absorpt_correction_T_min  0.8534
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            RED
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             3360
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.669
_refine_diff_density_min         -1.185
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.919
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1027
_refine_ls_number_reflns         17511
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.919
_refine_ls_R_factor_all          0.1847
_refine_ls_R_factor_gt           0.0657
_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^)+(0.0509P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1171
_refine_ls_wR_factor_ref         0.1550
_reflns_number_gt                7894
_reflns_number_total             17511
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3008844_si_002.cif
_cod_data_source_block           ims110m
_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.

'_exptl_absorpt_correction_type' value 'MULTI-SCAN'
changed to 'multi-scan' 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_cell_volume        7794.7(17)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4079614