Synthesis and Characterization of the First Mononuclear NiII Phosphorane Imino Complex
Laura Crociani; Francesco Tisato; Fiorenzo Refosco; Giuliano Bandoli; Benedetto Corain; Luigi M. Venanzi; Journal of the American Chemical Society 120 (1998) 2973–2974; doi:10.1021/ja9738440

data_4116710
_publ_contact_author
;
        Giuliano Bandoli
        Dipartimento di Scienze Farmaceutiche
        Universit. di Padova
        Via Marzolo 5
        35131 PADOVA
        Italy
;
_publ_contact_author_email       bandoli@pdfar3.dsfarm.unipd.it
_publ_contact_author_fax         'int.code +(49)8275345'
_publ_contact_author_phone       'int.code +(49)8275344'
_publ_section_title
;
 Synthesis and Characterization of the First Mononuclear NiII Phosphorane
 Imino Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2973
_journal_page_last               2974
_journal_paper_doi               10.1021/ja9738440
_journal_volume                  120
_journal_year                    1998
_chemical_formula_sum            'C24 H32 Cl F6 N Ni P4'
_chemical_formula_weight         666.55
_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                 110.17(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.464(4)
_cell_length_b                   12.007(4)
_cell_length_c                   18.518(5)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      11
_cell_volume                     3018.8(16)
_computing_cell_refinement       'R3 diffractometer software'
_computing_data_collection       'R3 diffractometer software'
_computing_data_reduction        'R3 diffractometer software'
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  'SHELXTL/PC(CIFTAB in SHELXL-93)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens Nicolet R3m/V diffractometer'
_diffrn_measurement_method       'omega scans '
_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  0.1018
_diffrn_reflns_av_sigmaI/netI    0.0504
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
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_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            4963
_diffrn_reflns_theta_max         24.06
_diffrn_reflns_theta_min         2.26
_diffrn_standards_decay_%        4
_diffrn_standards_interval_count 150
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.995
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       cuboids
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.584
_refine_diff_density_min         -0.985
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       0.0000(5)
_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   1.160
_refine_ls_goodness_of_fit_obs   1.190
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         4766
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.160
_refine_ls_restrained_S_obs      1.190
_refine_ls_R_factor_all          0.1080
_refine_ls_R_factor_obs          0.0627
_refine_ls_shift/esd_mean        0.037
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2022
_refine_ls_wR_factor_obs         0.1699
_reflns_number_observed          2555
_reflns_number_total             4766
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9738440.cif
_cod_data_source_block
J.Am.Chem.Soc.L.Crociani,F.Tisato,F.Refosco,G.Bandoli
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^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^)+(0.1000P)^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        3018.8(15)
_cod_database_code               4116710