1,3-Bis(trimethylsilyl)-2-phenyl-1-aza-3-phosphapropenide Anions as Bidentate Ligands for the Alkaline Earth Metals Magnesium, Calcium, Strontium, and Barium
Matthias Westerhausen; Matthias H. Digeser; Wolfgang Schwarz; Inorganic Chemistry 36 (1997) 521–527; doi:10.1021/ic960887t

data_4323312
_publ_section_title
;
 1,3-Bis(trimethylsilyl)-2-phenyl-1-aza-3-phosphapropenide Anions as
 Bidentate Ligands for the Alkaline Earth Metals Magnesium, Calcium,
 Strontium, and Barium
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              521
_journal_page_last               527
_journal_paper_doi               10.1021/ic960887t
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C34 H62 Ca N2 O2 P2 Si4'
_chemical_formula_weight         745.24
_chemical_name_systematic
;
 Bis(tetrahydrofuran)calcium =
bis[1,3-bis(trimethylsilyl)-2-phenyl-1-aza-3-phosphapropenide]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 92.53(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.228(7)
_cell_length_b                   12.792(5)
_cell_length_c                   23.140(10)
_cell_measurement_temperature    293(2)
_cell_volume                     4503(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.1131
_diffrn_reflns_av_sigmaI/netI    0.0970
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            1935
_diffrn_reflns_theta_max         15.00
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    0.345
_exptl_crystal_density_diffrn    1.099
_exptl_crystal_F_000             1608
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.056
_refine_ls_goodness_of_fit_obs   1.150
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         1725
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.129
_refine_ls_restrained_S_obs      1.182
_refine_ls_R_factor_all          0.1072
_refine_ls_R_factor_obs          0.0651
_refine_ls_shift/esd_max         -0.005
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0691P)^2^+9.9376P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1659
_refine_ls_wR_factor_obs         0.1392
_reflns_number_observed          1259
_reflns_number_total             1817
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960887t_2.cif
_cod_data_source_block           cancp;Compound2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0691P)^2^+9.9376P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0691P)^2^+9.9376P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4503.2(34)
_cod_database_code               4323312