Syntheses and structures of the first terminal phosphanylphosphido complex of hafnium [Cp(2)Hf(Cl){η(1)-(Me(3)Si)P-P(NEt(2))(2)}] and the first zirconocene-phosphanylphosphinidene dimer [Cp(2)Zr{μ(2)-P-P(NEt(2))(2)}(2)ZrCp(2)].
Grubba, Rafał; Wiśniewska, Aleksandra; Baranowska, Katarzyna; Matern, Eberhard; Pikies, Jerzy; Dalton transactions (Cambridge, England : 2003) 40 (2011) 2017–2024; doi:10.1039/c0dt01040e

data_7014662
_publ_section_title
;
 Syntheses and structures of the first terminal phosphanylphosphido
 complex of hafnium [Cp(2)Hf(Cl){\h(1)-(Me(3)Si)P-P(NEt(2))(2)}] and
 the first zirconocene-phosphanylphosphinidene dimer
 [Cp(2)Zr{\m(2)-P-P(NEt(2))(2)}(2)ZrCp(2)].
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2017
_journal_page_last               2024
_journal_paper_doi               10.1039/c0dt01040e
_journal_volume                  40
_journal_year                    2011
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C36 H60 N4 P4 Zr2'
_chemical_formula_sum            'C36 H60 N4 P4 Zr2'
_chemical_formula_weight         855.2
_chemical_name_common
;
Bis(mu-(bi(diethylamino)phosphinephosphinideno)-bis-
cyclopentadienylo zirconium(IV))
;
_chemical_name_systematic
;
Bis[\m-{bi(diethylamino)phosphinephosphinideno}-bis-cyclopentadienylo
zirconium(IV)]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2010-07-28
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
FM

2010-07-28 # Formatted by publCIF
;
_cell_angle_alpha                90
_cell_angle_beta                 105.17(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.309(2)
_cell_length_b                   12.521(3)
_cell_length_c                   19.225(6)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      11.2
_cell_measurement_theta_min      2.95
_cell_measurement_wavelength     0.71073
_cell_volume                     1930.4(9)
_computing_cell_refinement       'KM4 System (Ga\/ldecki, 1996)'
_computing_data_collection       'KM4 System (Ga\/ldecki, 1996)'
_computing_data_reduction        'DATAPROC (Ga\/ldecki, 1996)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia,1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS - 97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'KUMA KM4, serial detector'
_diffrn_measurement_method       \w--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_av_unetI/netI     0.1242
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            3917
_diffrn_reflns_theta_full        26.05
_diffrn_reflns_theta_max         26.05
_diffrn_reflns_theta_min         2.54
_diffrn_standards_decay_%        1.54
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.737
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.074
_refine_diff_density_min         -0.878
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         3801
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1477
_refine_ls_R_factor_gt           0.0586
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0943P)^2^+2.2757P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1432
_refine_ls_wR_factor_ref         0.1856
_reflns_number_gt                2231
_reflns_number_total             3801
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            C0DT01040E.TXT
_cod_data_source_block           raf3
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7014662