s-Block Metal Complexes of the Bis(tetramethylcyclopentadienyl) Phosphonium Diylide [Me(t-Bu)P(C5Me4)2]−
Brady, Erik D.; Chmely, Stephen C.; Jayaratne, Kumudini C.; Hanusa, Timothy P.; Young, Victor G.; Organometallics 27 (2008) 1612–; doi:10.1021/om700635c

data_4070545
_publ_section_title
;
 s-Block Metal Complexes of the Bis(tetramethylcyclopentadienyl)
 Phosphonium Diylide [Me(t-Bu)P(C5Me4)2]&#x2212;
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1612
_journal_paper_doi               10.1021/om700635c
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C27 H44 K O P'
_chemical_formula_weight         454.69
_chemical_name_common            01062a
_space_group_IT_number           14
_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                 113.760(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.3181(14)
_cell_length_b                   18.874(2)
_cell_length_c                   13.5474(17)
_cell_measurement_temperature    173(2)
_cell_volume                     2648.7(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0489
_diffrn_reflns_av_sigmaI/netI    0.0321
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            20264
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    0.276
_exptl_absorpt_correction_T_max  0.9401
_exptl_absorpt_correction_T_min  0.8851
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.03 (Sheldrick, 2000)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         4686
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0765P)^2^+1.6186P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1289
_refine_ls_wR_factor_ref         0.1337
_reflns_number_gt                4187
_reflns_number_total             4686
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700635c-file003.cif
_cod_data_source_block           01062a
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4070545