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_4089576
_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         'C18 H38 Cl3 N2 P Si Zr, C7 H8 '
_chemical_formula_sum            'C25 H46 Cl3 N2 P Si Zr'
_chemical_formula_weight         631.27
_chemical_name_common            'compound 3a'
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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                 90.771(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5679(2)
_cell_length_b                   13.1603(3)
_cell_length_c                   24.9054(5)
_cell_measurement_reflns_used    28172
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.29
_cell_measurement_theta_min      1.635
_cell_volume                     3135.72(12)
_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  0.0502
_diffrn_reflns_av_sigmaI/netI    0.0338
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            47277
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.79
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.712
_exptl_absorpt_correction_T_max  0.9406
_exptl_absorpt_correction_T_min  0.8389
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
[c.f. p. coppens,Crystallographic Computing ed F.R. Ahmed, 
S.R. Hall and C.P. Huber, Copenhagen, Munksgaard, (1970), 255-270]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.758
_refine_diff_density_min         -0.898
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         6658
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0278
_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^)+(0.0399P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0633
_refine_ls_wR_factor_ref         0.0662
_reflns_number_gt                5410
_reflns_number_total             6658
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om4005548_si_001.cif
_cod_data_source_block           cpd3a
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4089576