Deprotonated P-ylides As Templates for Novel Cyclopentadienyl Phosphonioalkyl, -alkylidene, and -alkylidyne (CpPC) Constrained-Geometry Complexes
Schröder, Fabian G.; Lichtenberg, Crispin; Elfferding, Michael; Sundermeyer, Jörg; Organometallics 32 (2013) 5082–; doi:10.1021/om4005548

data_4089581
_publ_section_title
;
 Deprotonated P-ylides As Templates for Novel Cyclopentadienyl
 Phosphonioalkyl, -alkylidene, and -alkylidyne (CpPC) Constrained-Geometry
 Complexes
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              5082
_journal_paper_doi               10.1021/om4005548
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C30 H45 P1 Si2 Zr1'
_chemical_formula_sum            'C30 H45 P Si2 Zr'
_chemical_formula_weight         584.03
_chemical_name_common            'compound 5d'
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                102.821(5)
_cell_angle_beta                 101.341(7)
_cell_angle_gamma                96.23(3)
_cell_formula_units_Z            2
_cell_length_a                   10.110(2)
_cell_length_b                   11.751(3)
_cell_length_c                   13.802(5)
_cell_measurement_reflns_used    19647
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.78
_cell_measurement_theta_min      1.26
_cell_volume                     1547.6(8)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'Diamond 3.0 (Brandenburg, 2004)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14887
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.76
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    0.501
_exptl_absorpt_correction_T_max  1.0883
_exptl_absorpt_correction_T_min  0.8626
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.752
_refine_diff_density_min         -1.361
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         6546
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0786P)^2^+0.4573P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1173
_reflns_number_gt                5274
_reflns_number_total             6546
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om4005548_si_001.cif
_cod_data_source_block           cpd5d
_cod_database_code               4089581