A new synthetic entry to phosphinophosphinidene complexes. Synthesis and structural characterisation of the first side-on bonded and the first terminally bonded phosphinophosphinidene zirconium complexes [mu-(1,2:2-eta-tBu2P=P)[Zr(Cl)Cp2]2] and [[Zr(PPhMe2)Cp2](eta1)-P-PtBu2)].
Pikies, Jerzy; Baum, Elke; Matern, Eberhard; Chojnacki, Jaroslaw; Grubba, Rafal; Robaszkiewicz, Andrzej; Chemical communications (Cambridge, England)  (2004) 2478–2479; doi:10.1039/b409673h

data_7113380
_publ_section_title
;
 A new synthetic entry to phosphinophosphinidene complexes. Synthesis and
 structural characterisation of the first side-on bonded and the first
 terminally bonded phosphinophosphinidene zirconium complexes
 [mu-(1,2:2-eta-tBu2P=P)[Zr(Cl)Cp2]2] and
 [[Zr(PPhMe2)Cp2](eta1)-P-PtBu2)].
;
_journal_issue                   21
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2478
_journal_page_last               2479
_journal_paper_doi               10.1039/b409673h
_journal_year                    2004
_chemical_formula_moiety         'C26 H39 P3 Zr'
_chemical_formula_sum            'C26 H39 P3 Zr'
_chemical_formula_weight         535.70
_chemical_name_common
;
Dicyclopentapdienylo(phenyldimethylphosphane)(eta$1!-di-tert-
butylphosphanylphosphinidene)zirconium
;
_chemical_name_systematic
;
Dicyclopentapdienylo(phenyldimethylphosphane)(\h^1^-
di-tert-butylphosphanylphosphinidene)zirconium
;
_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                78.91(3)
_cell_angle_beta                 87.11(3)
_cell_angle_gamma                85.26(3)
_cell_formula_units_Z            4
_cell_length_a                   9.312(2)
_cell_length_b                   11.574(2)
_cell_length_c                   25.220(5)
_cell_measurement_reflns_used    26
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      3.5
_cell_volume                     2656.6(9)
_computing_cell_refinement       'KM4 Oxford Diffraction'
_computing_data_collection       'KM4 Oxford Diffraction'
_computing_data_reduction        'DATAPROC Oxford Diffraction'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150.0(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'KM4 - Oxford Diffraction'
_diffrn_measurement_method       '\w - 2\q'
_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  0.0263
_diffrn_reflns_av_sigmaI/netI    0.0746
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10154
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        0.3
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.606
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
An attempt to perform the psi-scan absorption
correction led to worse structure parameters so we decided
not to apply it.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         2.032
_refine_diff_density_min         -1.693
_refine_diff_density_rms         0.241
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         9876
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.1659
_refine_ls_R_factor_gt           0.1011
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0989P)^2^+66.4172P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2533
_refine_ls_wR_factor_ref         0.3115
_reflns_number_gt                6887
_reflns_number_total             9876
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b409673h.txt
_cod_data_source_block           r1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_ambient_temperature' value '150(0.2)' was changed to
'150.0(2)' - precision was estimated.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        2656.7(9)
_cod_database_code               7113380