Structural Properties and Dynamics of Five-Coordinate Nickel(II)−π-Allyl Complexes Containing Monodentate Phosphorus Ligands
Rufińska, Anna; Goddard, Richard; Weidenthaler, Claudia; Bühl, Michael; Pörschke, Klaus-Richard; Organometallics 25 (2006) 2308–; doi:10.1021/om0601807

data_4075274
_publ_section_title
;
 Structural Properties and Dynamics of Five-Coordinate
 Nickel(II)&#x2212;\p-Allyl Complexes Containing Monodentate Phosphorus
 Ligands
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2308
_journal_paper_doi               10.1021/om0601807
_journal_volume                  25
_journal_year                    2006
_chemical_compound_source        tetrahydrofuran
_chemical_formula_moiety         'C12 H32 Ni P3 1+, C F3 O3 S 1-'
_chemical_formula_sum            'C13 H32 F3 Ni O3 P3 S'
_chemical_formula_weight         477.07
_chemical_name_systematic
; 
 tris(trimethylphosphine)(\h^3^-allyl)nickel(ii)
 trifluoromethanesulfonate 
;
_chemical_temperature_decomposition_gt 395
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                89.967(5)
_cell_angle_beta                 76.814(6)
_cell_angle_gamma                89.988(11)
_cell_formula_units_Z            2
_cell_length_a                   8.7689(12)
_cell_length_b                   10.4345(7)
_cell_length_c                   12.294(2)
_cell_measurement_reflns_used    15196
_cell_measurement_temperature    100
_cell_measurement_theta_max      33.14
_cell_measurement_theta_min      2.04
_cell_volume                     1095.2(2)
_computing_cell_refinement       'Denzo / Scalepack (Otwinowski 1997)'
_computing_data_collection       'Collect software (Nonius, 1998)'
_computing_data_reduction        'Denzo / Scalepack (Otwinowski 1997)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'CCD \w-scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         '0.3 mm focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_sigmaI/netI    0.0700
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11402
_diffrn_reflns_theta_full        33.13
_diffrn_reflns_theta_max         33.13
_diffrn_reflns_theta_min         2.39
_diffrn_standards_decay_%        0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.233
_exptl_absorpt_correction_T_max  0.95232
_exptl_absorpt_correction_T_min  0.83709
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'XPREP, Siemens (1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       plate
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.594
_refine_diff_density_min         -0.897
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         7888
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0001P)^2^+0.6596P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.0942
_reflns_number_gt                7008
_reflns_number_total             7888
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om0601807si20060223_123256.cif
_cod_data_source_block           1a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_temperature_decomposition_gt' since the value was
specified 'more than' ('>') a certain temperature. The value '>395
decomposition' was changed to '395' - it should be numeric and
without a unit designator.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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 
;
_cod_database_code               4075274