Bi- and Tricyclic Penta- and Hexacoordinated Phosphoranes with Varying Ring Sizes: Synthesis, Structures, and Reactivity
Musa A. Said; Melanie Pülm; Regine Herbst-Irmer; Kumara K. C. Swamy; Journal of the American Chemical Society 118 (1996) 9841–9849; doi:10.1021/ja960554v

data_4117182
_publ_contact_author
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      Dr. Regine Herbst-Irmer
      Institut f\"ur Anorganische Chemie
      Universit\"at G\"ottingen
      Tammannstr. 4
      37077 G\"ottingen
      Germany
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_publ_contact_author_email       rherbst@shelx.uni-ac.gwdg.de
_publ_contact_author_fax         '049 551 392582'
_publ_contact_author_phone       '049 551 393007'
_publ_section_title
;
 Bi- and Tricyclic Penta- and Hexacoordinated Phosphoranes with Varying
 Ring Sizes: Synthesis, Structures, and Reactivity
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9841
_journal_page_last               9849
_journal_paper_doi               10.1021/ja960554v
_journal_volume                  118
_journal_year                    1996
_chemical_formula_sum            'C52 H69 N O5.5 P'
_chemical_formula_weight         827.05
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                110.05(1)
_cell_angle_beta                 101.77(2)
_cell_angle_gamma                92.94(1)
_cell_formula_units_Z            4
_cell_length_a                   10.988(3)
_cell_length_b                   21.980(5)
_cell_length_c                   22.108(5)
_cell_measurement_reflns_used    46
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     4868(2)
_computing_cell_refinement       'Stoe DIF4'
_computing_data_collection       'Stoe DIF4'
_computing_data_reduction        'Stoe REDU4'
_computing_molecular_graphics    'Siemens SHELXTL-Plus'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measurement_device
'Stoe-Siemens-Huber four-circle-diffractometer'
_diffrn_measurement_method       'Profile data from 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  0.3520
_diffrn_reflns_av_sigmaI/netI    0.0656
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17857
_diffrn_reflns_theta_max         25.22
_diffrn_reflns_theta_min         3.53
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  90
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.103
_exptl_crystal_colour            pale_yellow
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.70
_exptl_crystal_size_min          0.60
_refine_diff_density_max         .871
_refine_diff_density_min         -.448
_refine_diff_density_rms         .066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.020
_refine_ls_goodness_of_fit_obs   1.048
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1213
_refine_ls_number_reflns         17477
_refine_ls_number_restraints     399
_refine_ls_restrained_S_all      1.045
_refine_ls_restrained_S_obs      1.055
_refine_ls_R_factor_all          0.1236
_refine_ls_R_factor_obs          0.0732
_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^)+( 0.1003P)^2^+5.6348P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2256
_refine_ls_wR_factor_obs         0.1768
_reflns_number_observed          10877
_reflns_number_total             17492
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja960554v_1.cif
_cod_data_source_block           k34
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.1003P)^2^+5.6348P] 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^)+( 0.1003P)^2^+5.6348P] 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        4867.5(21)
_cod_original_formula_sum        'C52 H69 N O5.50 P'
_cod_database_code               4117182