Polycyclic Bis(tert-butylamido)cyclodiphosph(III)azane Complexes of Lithium and Magnesium: Their Syntheses, Molecular Structures, and Relationships to Isoelectronic Cyclodisilazane Derivatives
Ingo Schranz; Lothar Stahl; Richard J. Staples; Inorganic Chemistry 37 (1998) 1493–1498; doi:10.1021/ic971201f

data_4322726
_publ_section_title
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 Polycyclic Bis(tert-butylamido)cyclodiphosph(III)azane Complexes of
 Lithium and Magnesium: Their Syntheses, Molecular Structures, and
 Relationships to Isoelectronic Cyclodisilazane Derivatives
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1493
_journal_page_last               1498
_journal_paper_doi               10.1021/ic971201f
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C24 H52 Mg N4 O2 P2'
_chemical_formula_weight         514.95
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.47
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6272(4)
_cell_length_b                   17.6643(7)
_cell_length_c                   16.3625(6)
_cell_measurement_reflns_used    201
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      19.95
_cell_measurement_theta_min      2.62
_cell_volume                     3071.5(2)
_computing_cell_refinement       'SMART (SIEMENS, V4.033, 1994)'
_computing_data_collection       'ASTRO (SIEMENS, V4.033, 1994)'
_computing_data_reduction        'SAINT (SIEMENS, V4.035, 1994)'
_computing_molecular_graphics    'SHELXTL (SIEMENS, 1994, ver 5.04)'
_computing_publication_material  'CIFTAB (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Siemens CCD'
_diffrn_measurement_method       '\w, 0.3 deg'
_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  0.0417
_diffrn_reflns_av_sigmaI/netI    0.0623
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            12015
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         1.70
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.187
_exptl_absorpt_correction_T_max  0.970459
_exptl_absorpt_correction_T_min  0.695488
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.114
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.801
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.125
_refine_ls_goodness_of_fit_obs   1.232
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4988
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.125
_refine_ls_restrained_S_obs      1.232
_refine_ls_R_factor_all          0.1084
_refine_ls_R_factor_obs          0.0797
_refine_ls_shift/esd_max         -0.006
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1034P)^2^+6.9416P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2392
_refine_ls_wR_factor_obs         0.2212
_reflns_number_observed          3609
_reflns_number_total             4988
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic971201f_3.cif
_cod_data_source_block           ls7f_Compound_3
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1034P)^2^+6.9416P] 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^)+(0.1034P)^2^+6.9416P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4322726