Separating the Racemic and Meso Diastereomers of a Binucleating Tetraphosphine Ligand System through the Use of Nickel Chloride
David A. Aubry; Scott A. Laneman; Frank R. Fronczek; George G. Stanley; Inorganic Chemistry 40 (2001) 5036–5041; doi:10.1021/ic010035f

data_4320241
_publ_section_title
;
 Separating the Racemic and Meso Diastereomers of a Binucleating
 Tetraphosphine Ligand System through the Use of Nickel Chloride
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5036
_journal_page_last               5041
_journal_paper_doi               10.1021/ic010035f
_journal_volume                  40
_journal_year                    2001
_chemical_compound_source        'local laboratory'
_chemical_formula_moiety         'C27 H40 N2 P4 Ni, C4 H8 O'
_chemical_formula_sum            'C31 H48 N2 Ni O P4'
_chemical_formula_weight         647.35
_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'
_cell_angle_alpha                90
_cell_angle_beta                 98.78(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.128(2)
_cell_length_b                   11.085(2)
_cell_length_c                   20.663(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      15.0
_cell_volume                     3424.5(9)
_computing_cell_refinement       CAD4_(Enraf-Nonius,_1994)
_computing_data_collection       CAD4_(Enraf-Nonius,_1994)
_computing_data_reduction        process_MolEN_(Fair,_1990)
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  BTABLE_PTABLE_CIF_IN_MolEN_(Fair,_1990)
_computing_structure_refinement  LSFM_MolEN_(Fair,_1990)
_computing_structure_solution    Direct_methods_(MULTAN,_Main_et_al.,_1980)
_diffrn_ambient_temperature      296
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           Cu-K\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.030
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            5586
_diffrn_reflns_theta_max         60.0
_diffrn_reflns_theta_min         2.5
_diffrn_standards_decay_%        10.1
_diffrn_standards_interval_time  166
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.80
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.820
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_density_method    none
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.58
_refine_diff_density_min         -0.05
_refine_ls_abs_structure_details ' ?'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.608
_refine_ls_goodness_of_fit_obs   1.737
_refine_ls_hydrogen_treatment    'calculated U=1.3xbonding atom'
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     331
_refine_ls_number_reflns         2679
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.063
_refine_ls_R_factor_obs          0.063
_refine_ls_shift/esd_max         0.100
_refine_ls_shift/esd_mean        0
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 4Fo^2^/(\s^2^(Fo^2^) + 0.0036 Fo^4^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.109
_refine_ls_wR_factor_obs         0.084
_reflns_number_observed          2679
_reflns_number_total             5379
_reflns_observed_criterion       >3.0\s(I)
_cod_data_source_file            ic010035f_1.cif
_cod_data_source_block           3r_thf
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '4Fo^2^/(\s^2^(Fo^2^) + 0.0036
Fo^4^)' was changed to 'calc'. New tag '_refine_ls_weighting_details'
was created. The value of the new tag was set to 'w =
4Fo^2^/(\s^2^(Fo^2^) + 0.0036 Fo^4^)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3424(1)
_cod_original_formula_sum        'C31 H48 N2 O1 P4 Ni'
_cod_database_code               4320241