Catalytic applications of keto-stabilised phosphorus ylides based on a macrocyclic scaffold: calixarenes with one or two pendant Ni(P,O)-subunits as ethylene oligomerisation and polymerisation catalysts.
Kuhn, Pierre; Sémeril, David; Jeunesse, Catherine; Matt, Dominique; Lutz, Pierre J.; Louis, Rémy; Neuburger, Markus; Dalton transactions (Cambridge, England : 2003)  (2006) 3647–3659; doi:10.1039/b603861a

data_7007344
_publ_section_title
;
 Catalytic applications of keto-stabilised phosphorus ylides based on a
 macrocyclic scaffold: calixarenes with one or two pendant
 Ni(P,O)-subunits as ethylene oligomerisation and polymerisation
 catalysts.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3647
_journal_page_last               3659
_journal_paper_doi               10.1039/b603861a
_journal_year                    2006
_chemical_formula_moiety         'C76.50 H75 Cl O8 P2'
_chemical_formula_sum            'C76.5 H75 Cl O8 P2'
_chemical_formula_weight         1219.75
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_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                86.82(5)
_cell_angle_beta                 83.22(5)
_cell_angle_gamma                78.40(5)
_cell_formula_units_Z            2
_cell_length_a                   10.127(2)
_cell_length_b                   16.167(2)
_cell_length_c                   20.818(4)
_cell_measurement_reflns_used    37021
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     3313.7(12)
_computing_cell_refinement       'Denzo (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo (Nonius B.V., 1998)'
_computing_molecular_graphics    'PLATON 98 (Spek, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\p 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1884
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            19356
_diffrn_reflns_theta_full        30.06
_diffrn_reflns_theta_max         30.06
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    0.162
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1290
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.094
_refine_diff_density_min         -0.990
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     767
_refine_ls_number_reflns         19355
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.2185
_refine_ls_R_factor_gt           0.0927
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0150P)^2^+7.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1949
_refine_ls_wR_factor_ref         0.2343
_reflns_number_gt                10532
_reflns_number_total             19355
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b603861a.txt
_cod_data_source_block           welt8
_cod_original_cell_volume        3313.6(10)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C76.50 H75 Cl O8 P2'
_cod_database_code               7007344