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_4323970
_publ_section_title
;
 Metal Complexes of Mesitylphosphine: Synthesis, Structure, and
 Spectroscopy
;
_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            'C36 H52 Ni P4'
_chemical_formula_weight         667.37
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 115.84(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.584(4)
_cell_length_b                   11.506(2)
_cell_length_c                   18.965(4)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      7.5
_cell_volume                     3650(2)
_computing_cell_refinement       P4
_computing_data_collection       P4
_computing_data_reduction        XDISK
_computing_molecular_graphics    XP
_computing_publication_material  XPUBL
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      252(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       Wyckoff
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1127
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3894
_diffrn_reflns_theta_max         21.00
_diffrn_reflns_theta_min         2.04
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.730
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Yellow-Green
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_description       Block
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.670
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.97
_refine_ls_goodness_of_fit_obs   1.56
_refine_ls_hydrogen_treatment    ignored
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         3894
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.97
_refine_ls_restrained_S_obs      1.56
_refine_ls_R_factor_all          0.1489
_refine_ls_R_factor_obs          0.0900
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w=1/[\s^2^(Fo)+(0.001F^2^)]
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2671
_refine_ls_wR_factor_obs         0.1064
_reflns_number_observed          2148
_reflns_number_total             3894
_reflns_observed_criterion       >4.5sigma(F)
_cod_data_source_file            ic960529q_2.cif
_cod_data_source_block           glu4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo)+(0.001F^2^)]' 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)+(0.001F^2^)]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3649.8(141)
_cod_database_code               4323970