Metal Complexes of Mesitylphosphine: Synthesis, Structure, and Spectroscopy
Igor V. Kourkine; Stanislav V. Maslennikov; Robert Ditchfield; David S. Glueck; Glenn P. A. Yap; Louise M. Liable-Sands; Arnold L. Rheingold; Inorganic Chemistry 35 (1996) 6708–6716; doi:10.1021/ic960529q

data_4323972
_publ_section_title
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 Metal Complexes of Mesitylphosphine: Synthesis, Structure, and
 Spectroscopy
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6708
_journal_page_last               6716
_journal_paper_doi               10.1021/ic960529q
_journal_volume                  35
_journal_year                    1996
_chemical_formula_sum            'C50 H52 Ni P4'
_chemical_formula_weight         835.51
_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
_cell_angle_alpha                102.315(7)
_cell_angle_beta                 90.921(9)
_cell_angle_gamma                114.15(1)
_cell_formula_units_Z            2
_cell_length_a                   9.587(1)
_cell_length_b                   11.528(1)
_cell_length_c                   22.194(2)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      7.5
_cell_volume                     2171.9(4)
_computing_cell_refinement       XSCANS
_computing_data_collection       XSCANS
_computing_data_reduction        XPREP
_computing_molecular_graphics    XP
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       omega
_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  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0503
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            6824
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.35
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.628
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_description       block
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       0.0023(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.204
_refine_ls_goodness_of_fit_obs   1.318
_refine_ls_hydrogen_treatment    'idealized contribution'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         5596
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.211
_refine_ls_restrained_S_obs      1.318
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_obs          0.0414
_refine_ls_shift/esd_max         -0.006
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1121
_refine_ls_wR_factor_obs         0.1075
_reflns_number_observed          4416
_reflns_number_total             5611
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960529q_4.cif
_cod_data_source_block           glu18
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.0000P] 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^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2172.0(4)
_cod_database_code               4323972