Double Phosphaalkyne Insertion to a Tungsten Alkylidene: Formation of a Diphosphametallabicyclobutane
Jamison, Gregory M.; Wheeler, David R.; Loy, Douglas A.; Ziller, Joseph W.; Organometallics 24 (2005) 2245–2247; doi:10.1021/om050150o

data_1100871
_publ_section_title
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 Double Phosphaalkyne Insertion to a Tungsten Alkylidene:&#x2009;
 Formation of a Diphosphametallabicyclobutane
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_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2245
_journal_page_last               2247
_journal_paper_doi               10.1021/om050150o
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C35 H51 F12 N O2 P2 W'
_chemical_formula_weight         991.56
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 117.670(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   42.110(5)
_cell_length_b                   10.6323(9)
_cell_length_c                   20.577(2)
_cell_measurement_reflns_used    37
_cell_measurement_temperature    163
_cell_measurement_theta_max      11.70
_cell_measurement_theta_min      5.10
_cell_volume                     8159.4(14)
_diffrn_ambient_temperature      163
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0393
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            5419
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        '< 1.0'
_diffrn_standards_interval_count 99
_diffrn_standards_interval_time  ?
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    2.996
_exptl_absorpt_correction_T_max  0.6052
_exptl_absorpt_correction_T_min  0.4794
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3968
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.17
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.060
_refine_ls_goodness_of_fit_obs   1.085
_refine_ls_hydrogen_treatment    ?
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         5325
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_restrained_S_obs      1.085
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_obs          0.0317
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+57.0484P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0714
_refine_ls_wR_factor_obs         0.0650
_reflns_number_observed          4385
_reflns_number_total             5334
_reflns_observed_criterion       >2sigma(I)
_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_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/a' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+57.0484P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+57.0484P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               1100871