Structural characterisation of cationic methylallyl, methylindenyl and pentamethylcyclopentadienyl nickel complexes containing the bulky phosphine 1,2-bis(diisopropylphosphino)ethane †
Tenorio, Manuel Jiménez; Puerta, M. Carmen; Salcedo, Isabel; Valerga, Pedro; Journal of the Chemical Society, Dalton Transactions  (2001) 653–; doi:10.1039/b008441g

data_7702486
_publ_section_title
;
 Structural characterisation of cationic methylallyl, methylindenyl and
 pentamethylcyclopentadienyl nickel complexes containing the bulky
 phosphine 1,2-bis(diisopropylphosphino)ethane&#x200A;&#x2020;
;
_journal_issue                   5
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              653
_journal_paper_doi               10.1039/b008441g
_journal_year                    2001
_chemical_formula_sum            'C48.83 H63.66 B Cl1.66 Ni P2'
_chemical_formula_weight         854.40
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.65(2)
_cell_angle_beta                 105.09(2)
_cell_angle_gamma                94.31(2)
_cell_formula_units_Z            2
_cell_length_a                   13.252(3)
_cell_length_b                   16.619(4)
_cell_length_c                   10.964(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.3
_cell_measurement_theta_min      12.6
_cell_volume                     2271.8(13)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_molecular_graphics    'ORTEP32 (L.J.Farrugia, 1999)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    DIRDIF
_diffrn_ambient_temperature      290(2)
_diffrn_measured_fraction_theta_full 0.844
_diffrn_measured_fraction_theta_max 0.844
_diffrn_measurement_device_type  AFC6S
_diffrn_measurement_method       'omega/2-theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1164
_diffrn_reflns_av_sigmaI/netI    0.0797
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7090
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.52
_diffrn_standards_decay_%        negligible
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.647
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.880
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   psi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             908.00
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.995
_refine_diff_density_min         -1.279
_refine_diff_density_rms         0.246
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.261
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         6792
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.261
_refine_ls_R_factor_all          0.1460
_refine_ls_R_factor_gt           0.1025
_refine_ls_shift/su_max          1.205
_refine_ls_shift/su_mean         0.123
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1803P)^2^+1.2460P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2966
_refine_ls_wR_factor_ref         0.3924
_reflns_number_gt                4490
_reflns_number_total             6792
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b008441g.txt
_cod_data_source_block           '[(MeIn)Ni(dippe)][BPh4]0.83_Cl2CH2'
_cod_original_cell_volume        2271.9(13)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7702486