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_7014663
_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         'C21 H39 Cl Hf N2 P2 Si'
_chemical_formula_sum            'C21 H39 Cl Hf N2 P2 Si'
_chemical_formula_weight         623.51
_chemical_name_common
;
((Bis-
diethylaminophosphanyl)(trimethylsilyl)phosphide)(chlorido) (bis-
cyclopentadienylo) hafnium(IV)
;
_chemical_name_systematic
;
{(Bis-diethylaminophosphanyl)(trimethylsilyl)phosphide}(chlorido)
(bis-cyclopentadienylo)
hafnium(IV)

;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_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             2010-07-31
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
FM

2010-08-03 # Formatted by publCIF
;
_cell_angle_alpha                71.665(14)
_cell_angle_beta                 78.786(13)
_cell_angle_gamma                81.294(13)
_cell_formula_units_Z            4
_cell_length_a                   11.0239(17)
_cell_length_b                   15.008(2)
_cell_length_c                   16.892(3)
_cell_measurement_reflns_used    7306
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      32.4603
_cell_measurement_theta_min      2.2163
_cell_measurement_wavelength     0.71073
_cell_volume                     2590.0(7)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2006)

;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2006)

;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction, 2006)

;
_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, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.1883
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type
'Goniometer KM4/Xcalibur, detector: Sapphire2 (large Be window)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0194156347
_diffrn_orient_matrix_UB_12      -0.0309675403
_diffrn_orient_matrix_UB_13      0.0377883531
_diffrn_orient_matrix_UB_21      -0.0436564862
_diffrn_orient_matrix_UB_22      0.0251161659
_diffrn_orient_matrix_UB_23      0.0242163641
_diffrn_orient_matrix_UB_31      -0.0457491499
_diffrn_orient_matrix_UB_32      -0.030150535
_diffrn_orient_matrix_UB_33      0.0032727192
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0962
_diffrn_reflns_av_unetI/netI     0.1169
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17964
_diffrn_reflns_theta_full        25.5
_diffrn_reflns_theta_max         25.5
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    4.311
_exptl_absorpt_correction_T_max  0.622
_exptl_absorpt_correction_T_min  0.425
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED (Oxford Diffraction, 2006)

;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.1707
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.0538
_refine_diff_density_max         3.06
_refine_diff_density_min         -1.775
_refine_diff_density_rms         0.315
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         17964
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.1372
_refine_ls_R_factor_gt           0.0836
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1587P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2156
_refine_ls_wR_factor_ref         0.2462
_reflns_number_gt                11025
_reflns_number_total             17964
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            C0DT01040E.TXT
_cod_data_source_block           ola1k
_cod_database_code               7014663