Fluoride Displacement by Lithium Reagents. An Improved Method for the Synthesis of Nickel Hydroxo, Alkoxo, and Amido Complexes
Cámpora, Juan; Matas, Inmaculada; Palma, Pilar; Graiff, Claudia; Tiripicchio, Antonio; Organometallics 24 (2005) 2827–; doi:10.1021/om0489709

data_4075639
_publ_section_title
;
 Fluoride Displacement by Lithium Reagents. An Improved Method for the
 Synthesis of Nickel Hydroxo, Alkoxo, and Amido Complexes
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2827
_journal_paper_doi               10.1021/om0489709
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C15 H35 F Ni P2'
_chemical_formula_weight         355.08
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 96.02(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.727(3)
_cell_length_b                   13.228(5)
_cell_length_c                   18.666(5)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      36
_cell_measurement_theta_min      18
_cell_volume                     1897.4(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Enraf Nonius CAD 4'
_diffrn_measurement_method       '\q/2\q scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0192
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2757
_diffrn_reflns_theta_full        60.00
_diffrn_reflns_theta_max         60.00
_diffrn_reflns_theta_min         4.10
_diffrn_standards_interval_count 100
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    3.034
_exptl_absorpt_correction_T_max  0.7354
_exptl_absorpt_correction_T_min  0.2023
_exptl_absorpt_correction_type   refdelf
_exptl_crystal_colour            ?????
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.933
_refine_diff_density_min         -1.063
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2757
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0581
_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^)+(0.1383P)^2^+1.8235P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1701
_refine_ls_wR_factor_ref         0.1890
_reflns_number_gt                2488
_reflns_number_total             2757
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0489709si20041230_064710.cif
_cod_data_source_block           Compound_1b
_cod_original_cell_volume        1897.4(11)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4075639