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_7113379
_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         'C28 H38 Cl2 P2 Zr2'
_chemical_formula_sum            'C28 H38 Cl2 P2 Zr2'
_chemical_formula_weight         689.86
_chemical_name_common
;
(mu- (1,2:2 - eta - 1,1-ditertbutyldiphosphene)
bis(dicyclopentadienatochlorozirconium))
;
_chemical_name_systematic
;
[\m- (1,2:2 - \h - 1,1-ditertbutyldiphosphene)
bis(dicyclopentadienatochlorozirconium)]
;
_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                 102.026(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7489(4)
_cell_length_b                   23.9432(10)
_cell_length_c                   11.5529(5)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      27.15
_cell_measurement_theta_min      1.70
_cell_volume                     2908.0(2)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    SCHAKAL
_computing_publication_material  SHELX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector                 'images plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_details      ' 276 frames, detector distance = 120 mm'
_diffrn_measurement_device       '2-circle- goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_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  0.0422
_diffrn_reflns_av_sigmaI/netI    0.0299
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15035
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.70
_diffrn_source_current           40
_diffrn_source_power             1.80
_diffrn_source_voltage           45
_exptl_absorpt_coefficient_mu    1.026
_exptl_absorpt_correction_T_max  0.6922
_exptl_absorpt_correction_T_min  0.4829
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         5063
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0206
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0242P)^2^+1.1609P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0530
_refine_ls_wR_factor_ref         0.0539
_reflns_number_gt                4713
_reflns_number_total             5063
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b409673h.txt
_cod_data_source_block           pik2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7113379