Unusual addition reactions of lithium alkoxides to 2,4,6-tri-tert-butyl-1,3,5-triphosphabenzene
Krein, M.; Bergsträßer, U.; Peters, C.; Ruf, S. G.; Regitz, M.; Chemical Communications  (2000) 2015–; doi:10.1039/b006795o

data_7111108
_publ_section_title
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 Unusual addition reactions of lithium alkoxides to
 2,4,6-tri-tert-butyl-1,3,5-triphosphabenzene
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_journal_issue                   20
_journal_name_full               'Chemical Communications'
_journal_page_first              2015
_journal_paper_doi               10.1039/b006795o
_journal_year                    2000
_chemical_formula_sum            'C18 H39 O3 P3'
_chemical_formula_weight         396.40
_chemical_melting_point          51
_chemical_name_systematic
;
2,4,6-tri-tert-butyl-1,3,5-methoxy-1,3,5-triphosphacyclohexane
;
_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                 111.90(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.384(2)
_cell_length_b                   24.807(5)
_cell_length_c                   10.901(2)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max
;
5000 quasi-centered reflections selected from the whole data
were selected with the program SELECT 2.87 (Fa. STOE, 1998)
;
_cell_volume                     2354.5(10)
_computing_cell_refinement       'STOE-CELL 2.87 (STOE-1998)'
_computing_data_collection       'STOE-EXPOSE 2.87 (STOE-1998)'
_computing_data_reduction        'STOE-INTEGRATE 2.87 (STOE-1998)'
_computing_molecular_graphics    'SHELXTL-PLUS Siemens Ver. 5.03'
_computing_publication_material  'SHELXTL-PLUS Siemens Ver. 5.03'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       STOE-IPDS-diffractometer
_diffrn_measurement_method
;
167 exposures were taken in the 0-200 phi range with a crystal to 
detector distance of 80 mm and an exposure time of 3.00 minutes.
Dynamic profiles (17-21 pixels) were used for integration.
;
_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  0.0579
_diffrn_reflns_av_sigmaI/netI    0.0373
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            15039
_diffrn_reflns_theta_max         24.12
_diffrn_reflns_theta_min         2.59
_diffrn_standards_number
;
At least 50 reflections with a I/s(I) > 6 taken from each frame were
used to calculate the decay.
;
_exptl_absorpt_coefficient_mu    0.265
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_description       prism
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.223
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.279
_refine_ls_goodness_of_fit_obs   1.437
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         3635
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.325
_refine_ls_restrained_S_obs      1.437
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_obs          0.0478
_refine_ls_shift/esd_max         0.208
_refine_ls_shift/esd_mean        0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+0.0804P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1315
_refine_ls_wR_factor_obs         0.1223
_reflns_number_observed          2731
_reflns_number_total             3641
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b006795osup1.cif
_cod_data_source_block           krein
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+0.0804P] 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^)+(0.0580P)^2^+0.0804P] 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_original_cell_volume        2354.8(8)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7111108