Syntheses and Structures of [(THF)nM{(NSiMe3)2PPh2}2] Complexes (M = Be, Mg, Ca, Sr, Ba;n= 0-2): Deviation of Alkaline Earth Metal Cations from the Plane of an Anionic Ligand
Roland Fleischer; Dietmar Stalke; Inorganic Chemistry 36 (1997) 2413–2419; doi:10.1021/ic9613117

data_4323450
_publ_contact_author             'Prof. Dr. Dietmar Stalke'
_publ_contact_author_email       dstalke@chemie.uni-wuerzburg.de
_publ_section_title
;
 Syntheses and Structures of [(THF)nM{(NSiMe3)2PPh2}2] Complexes (M = Be,
 Mg, Ca, Sr, Ba;n= 0-2): Deviation of Alkaline Earth Metal Cations from
 the Plane of an Anionic Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2413
_journal_page_last               2419
_journal_paper_doi               10.1021/ic9613117
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C36 H56 Be N4 P2 Si4'
_chemical_formula_weight         728.16
_chemical_melting_point          140
_chemical_name_systematic
;
 Berylium-N,N'-Bis(trimethylsilyl)-aminodiphenylphosphinimid
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 100.92(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.845(8)
_cell_length_b                   11.474(3)
_cell_length_c                   19.836(8)
_cell_measurement_reflns_used    58
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     4211(3)
_computing_cell_refinement       DIF4
_computing_data_collection       DIF4
_computing_data_reduction        REDU4
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  SHELXTL-Plus
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measurement_device       STOE-AED
_diffrn_measurement_method       'profile fitted on 2theta/omega'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0144
_diffrn_reflns_av_sigmaI/netI    0.0192
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7910
_diffrn_reflns_theta_max         22.57
_diffrn_reflns_theta_min         4.06
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  90
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.246
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.5
_refine_diff_density_max         .159
_refine_diff_density_min         -.201
_refine_diff_density_rms         .030
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.45(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.032
_refine_ls_goodness_of_fit_obs   1.041
_refine_ls_hydrogen_treatment    riding-model
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         5515
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.032
_refine_ls_restrained_S_obs      1.040
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_obs          0.0264
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.0395P)^2^+1.3980P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0671
_refine_ls_wR_factor_obs         0.0658
_reflns_number_observed          5233
_reflns_number_total             5515
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9613117_2.cif
_cod_data_source_block           berta
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0395P)^2^+1.3980P] 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^)+( 0.0395P)^2^+1.3980P] 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        4211.4(27)
_cod_database_code               4323450