Schulz‒Flory oligomerisation of ethylene by the binuclear nickel(II) complex Ni2Cl4[cis,trans,cis-1,2,3,4-tetrakis-(diphenylphosphino)cyclobutane]
Claudio Bianchini; Luca Gonsalvi; Werner Oberhauser; David Sémeril; Peter Brüggeller; Rene Gutmann; Dalton Trans.  (2003) 3869–3875; doi:10.1039/b308388h

data_7013459
_publ_section_title
;
 Schulz--Flory oligomerisation of ethylene by the binuclear nickel(II)
 complex
 Ni2Cl4[cis,trans,cis-1,2,3,4-tetrakis-(diphenylphosphino)cyclobutane]
;
_journal_issue                   20
_journal_name_full               'Dalton Trans.'
_journal_page_first              3869
_journal_page_last               3875
_journal_paper_doi               10.1039/b308388h
_journal_year                    2003
_chemical_formula_moiety         'C52 H44 Cl4 P4 Ni2 x 2 C3 H7 N O'
_chemical_formula_sum            'C58 H58 Cl4 N2 Ni2 O2 P4'
_chemical_formula_weight         1198.20
_chemical_name_common            (Ni2Cl4(cyclo-tetraphos))
_chemical_name_systematic        '[Ni2Cl4(cyclo-tetraphos)]'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.53(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.018(2)
_cell_length_b                   18.891(4)
_cell_length_c                   13.241(3)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.0
_cell_volume                     2850.3(11)
_computing_cell_refinement       'Software of the Siemens P4'
_computing_data_collection       'Siemens P4'
_computing_data_reduction        'Software of the Siemens P4'
_computing_molecular_graphics    'SHELXTL PLUS'
_computing_publication_material  'SHELXTL PLUS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       omega-scans
_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  0.038
_diffrn_reflns_av_sigmaI/netI    0.4668
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6861
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.002
_exptl_absorpt_correction_T_max  0.820
_exptl_absorpt_correction_T_min  0.653
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1252
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         5713
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.1028
_refine_ls_R_factor_gt           0.0595
_refine_ls_shift/su_max          -0.022
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0588P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1209
_refine_ls_wR_factor_ref         0.2035
_reflns_number_gt                1112
_reflns_number_total             5713
_reflns_threshold_expression     >3sigma(I)
_cod_data_source_file            b308388h.txt
_cod_data_source_block           '[Ni2Cl4(cyclo-tetraphos)]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'Psi-scans' was replaced
with 'psi-scan' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        2850.3(10)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7013459
_diffrn_measured_fraction        0.969