Reversal of polarization in amidophosphines: neutral- and anionic-kappaP coordination vs. anionic-kappaP,N coordination and the formation of nickelaazaphosphiranes.
Schranz, Ingo; Lief, Graham R.; Carrow, Christopher J.; Haagenson, Dana C.; Grocholl, Luke; Stahl, Lothar; Staples, Richard J.; Boomishankar, Ramamoorthy; Steiner, Alexander; Dalton transactions (Cambridge, England : 2003)  (2005) 3307–3318; doi:10.1039/b507040f

data_7000097
_publ_section_title
;
 Reversal of polarization in amidophosphines: neutral- and
 anionic-kappaP coordination vs. anionic-kappaP,N coordination and the
 formation of nickelaazaphosphiranes.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3307
_journal_page_last               3318
_journal_paper_doi               10.1039/b507040f
_journal_year                    2005
_chemical_formula_sum            'C33 H61 Cl N6 Ni P2 Si2'
_chemical_formula_weight         754.16
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.343(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6331(13)
_cell_length_b                   15.7716(15)
_cell_length_c                   25.212(2)
_cell_measurement_temperature    213(2)
_cell_volume                     4220.9(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0255
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            7138
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    0.685
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1616
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       0.0023(3)
_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_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         5506
_refine_ls_number_restraints     831
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0520
_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^)+(0.0754P)^2^+6.0279P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1397
_refine_ls_wR_factor_ref         0.1444
_reflns_number_gt                4971
_reflns_number_total             5506
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b507040f.txt
_cod_data_source_block           10
_cod_original_cell_volume        4220.8(8)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7000097