Synthesis, Reactivity, and Theoretical Studies of the η2(4e)-Bonded Phosphaalkyne Complex [CpMo{P(OMe)3}2{η2(4e)-P⋮CBut}][B(C6F5)4] and the Molybdenum-Mediated Cyclocotrimerization of Alkyne and Phosphaalkyne Ligands
Burrows, Andrew D.; Carr, Nicholas; Green, Michael; Lynam, Jason M.; Mahon, Mary F.; Murray, Martin; Kiran, Boggavarapu; Nguyen, Minh T.; Jones, Cameron; Organometallics 21 (2002) 3076–; doi:10.1021/om020169g

data_4076868
_publ_section_title
;
 Synthesis, Reactivity, and Theoretical Studies of the \h2(4e)-Bonded
 Phosphaalkyne Complex [CpMo{P(OMe)3}2{\h2(4e)-P&#x22EE;CBut}][B(C6F5)4]
 and the Molybdenum-Mediated Cyclocotrimerization of Alkyne and
 Phosphaalkyne Ligands
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3076
_journal_paper_doi               10.1021/om020169g
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C36.7 H33 F6 Mo O P3'
_chemical_formula_weight         792.88
_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                 104.41(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.526(3)
_cell_length_b                   11.326(3)
_cell_length_c                   23.276(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      12
_cell_volume                     3453.6(14)
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Enraf Nonius CAD4 diffractometer '
_diffrn_measurement_method       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_wavelength     0.70930
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0752
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4249
_diffrn_reflns_theta_full        21.99
_diffrn_reflns_theta_max         21.99
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    0.581
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_type   DIFABS
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1609
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.573
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         4249
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.1105
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0789P)^2^+15.4362P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1251
_refine_ls_wR_factor_ref         0.1524
_reflns_number_gt                2728
_reflns_number_total             4249
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om020169g.cif
_cod_data_source_block           xray
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

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_sg_symbol_H-M      P21/c
_cod_original_formula_sum        'C36.70 H33 F6 Mo O P3'
_cod_database_code               4076868