Anion effect in the diastereoselective formation of bischelated Ni(II) complexes with a novel, chiral phosphine derived from 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU)
O'Reilly, Matthew; Pattacini, Roberto; Braunstein, Pierre; Dalton Transactions  (2009) 6092–; doi:10.1039/b909329j

data_7001772
_publ_section_title
;
 Anion effect in the diastereoselective formation of bischelated Ni(II)
 complexes with a novel, chiral phosphine derived from
 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU)
;
_journal_issue                   31
_journal_name_full               'Dalton Transactions'
_journal_page_first              6092
_journal_paper_doi               10.1039/b909329j
_journal_year                    2009
_chemical_formula_moiety         'C42 H50 N4 Ni P2, 2(Br), 6(H2 O)'
_chemical_formula_sum            'C42 H62 Br2 N4 Ni O6 P2'
_chemical_formula_weight         999.43
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 90.227(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.9492(3)
_cell_length_b                   15.0496(5)
_cell_length_c                   25.3293(5)
_cell_measurement_reflns_used    27207
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     4554.9(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  PLATON
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_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  0.0525
_diffrn_reflns_av_sigmaI/netI    0.0706
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24227
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.70
_exptl_absorpt_coefficient_mu    2.299
_exptl_absorpt_correction_T_max  0.737
_exptl_absorpt_correction_T_min  0.641
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'L. Spek, J. Appl.Cryst. 2003, 36, 7, B. Blessing, Acta Cryst, 1995, A51, 33'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.680
_refine_diff_density_min         -2.091
_refine_diff_density_rms         0.111
_refine_ls_extinction_coef       0.0009(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   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     538
_refine_ls_number_reflns         10110
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1045
_refine_ls_R_factor_gt           0.0638
_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^)+(0.0759P)^2^+14.7638P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1576
_refine_ls_wR_factor_ref         0.1775
_reflns_number_gt                6827
_reflns_number_total             10110
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b909329j.txt
_cod_data_source_block           4.6H2O
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7001772