2-Phosphinophenolate Complexes: Formation and Crystal Structure of a Novel Trinuclear μ-O Nickel(II)-Tris(PO-Chelate)
Joachim Heinicke; Normen Peulecke; Konstantin Karaghiosoff; Peter Mayer; Inorganic Chemistry 44 (2005) 2137–2139; doi:10.1021/ic0484304

data_4308969
_publ_contact_author_address
;
Institut fuer Chemie und Biochemie
Universitaet Greifswald
D-17487 Greifswald
Germany
;
_publ_contact_author_email       heinicke@uni-greifswald.de
_publ_contact_author_fax         '+49 3834 864337'
_publ_contact_author_name        'Joachim Heinicke'
_publ_contact_author_phone       '+49 3834 864319'
_publ_section_title
;
2-Phosphinophenolate Complexes: Formation and Crystal Structure of a
Novel Trinuclear \m-O Nickel(II)-Tris(PO-Chelate)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2137
_journal_page_last               2139
_journal_paper_doi               10.1021/ic0484304
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'Ni, 2(Ni P3 O6 C57 H48), 6(O C4 H8)'
_chemical_formula_sum            'C138 H144 Ni3 O18 P6'
_chemical_formula_weight         2452.532
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_author_name               'Mayer, P.'
_audit_block_code                Ni3_C6H3OMeOPPh2_thf_fn340_klk
_audit_creation_date             25-Oct-01
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_audit_update_record             16-Jun-04
_cell_angle_alpha                90.00
_cell_angle_beta                 101.82(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.344(3)
_cell_length_b                   21.235(4)
_cell_length_c                   19.134(4)
_cell_measurement_reflns_used    81959
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.134
_cell_volume                     6102(2)
_computing_cell_refinement       'Collect (Nonius BV, 1997-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'Collect (Nonius BV, 1997-2000)'
_computing_molecular_graphics
;
ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid
Plot Program for Crystal Structure Illustrations, Oak Ridge National
Laboratory Report ORNL-6895, 1996). Windows version (L. J. Farrugia, Univ.
Glasgow) used --- SCHAKAL (E. Keller, University of  Freiburg (Breisgau),
Germany, 1995).
;
_computing_publication_material
;
PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version).
--- T.B.Cohen, Pure Appl. Chem. 1996,68,2339-2359 (atomic masses).
;
_computing_structure_refinement
'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'Kappa CCD'
_diffrn_measurement_device_type  '95mm CCD camera on \k-goniostat'
_diffrn_radiation_collimation    0.60
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0719
_diffrn_reflns_av_sigmaI/netI    0.0794
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            60037
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.18
_diffrn_source_current           75
_diffrn_source_power             4.125
_diffrn_source_type              'FR 591 generator'
_diffrn_source_voltage           55
_exptl_absorpt_coefficient_mu    0.604
_exptl_absorpt_correction_T_max  0.9328
_exptl_absorpt_correction_T_min  0.8988
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'Absorption correction with XRed, rev 1.09, STOE (Darmstadt, Germany)'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.3348(4)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2580
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.782
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     732
_refine_ls_number_reflns         13907
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1391
_refine_ls_R_factor_gt           0.0705
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1027P)^2^+4.1147P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1800
_refine_ls_wR_factor_ref         0.2145
_reflns_number_gt                7728
_reflns_number_total             13907
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0484304si20050228_123800.cif
_cod_data_source_block           fn340
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4308969