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_4089579
_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         'C22 H47 N2 P Si2 Zr'
_chemical_formula_sum            'C22 H47 N2 P Si2 Zr'
_chemical_formula_weight         517.99
_chemical_name_common            'compound 5a'
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yab'
_space_group_name_H-M_alt        'P 1 21/a 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 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                 92.553(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.4331(4)
_cell_length_b                   15.1972(3)
_cell_length_c                   13.9683(4)
_cell_measurement_reflns_used    33538
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.16
_cell_measurement_theta_min      1.46
_cell_volume                     2848.74(13)
_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    'SIR2004 (Giacovazzo et al, 2004)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            43532
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.74
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    0.537
_exptl_absorpt_correction_T_max  1.0869
_exptl_absorpt_correction_T_min  0.7123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.971
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.931
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         6035
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0293
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0531P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0741
_refine_ls_wR_factor_ref         0.0761
_reflns_number_gt                4833
_reflns_number_total             6035
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om4005548_si_001.cif
_cod_data_source_block           cpd5a
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               4089579