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_4070546
_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_moiety         'C29 H54 Ca N P Si2'
_chemical_formula_sum            'C29 H54 Ca N P Si2'
_chemical_formula_weight         543.69
_chemical_name_common            01022a
_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                 104.880(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.615(5)
_cell_length_b                   10.092(3)
_cell_length_c                   21.098(6)
_cell_measurement_reflns_used    1896
_cell_measurement_temperature    173(2)
_cell_volume                     3213.3(17)
_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  0.0462
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            23454
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    0.337
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.781724
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (R. Blessing, Acta Cryst. (1995))'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.124
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.738
_refine_diff_density_min         -0.319
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5678
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1257
_refine_ls_R_factor_gt           0.0464
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0568
_refine_ls_wR_factor_ref         0.1365
_reflns_number_gt                4713
_reflns_number_total             5678
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700635c-file004.cif
_cod_data_source_block           01022a
_cod_original_cell_volume        3213.2(16)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4070546