Cyclic Aminophosphites and -phosphoranes Possessing Six- and Higher-Membered Rings: A Comparative Study of Structure and Reactivity
Musa A. Said; Melanie Pülm; Regine Herbst-Irmer; K. C. Kumara Swamy; Inorganic Chemistry 36 (1997) 2044–2051; doi:10.1021/ic9611958

data_4323417
_publ_contact_author
;
      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
;
 Cyclic Aminophosphites and -phosphoranes Possessing Six- and
 Higher-Membered Rings: A Comparative Study of Structure and Reactivity
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2044
_journal_page_last               2051
_journal_paper_doi               10.1021/ic9611958
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C35 H54 N O2 P'
_chemical_formula_weight         551.76
_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                96.97(2)
_cell_angle_beta                 103.96(2)
_cell_angle_gamma                96.53(2)
_cell_formula_units_Z            2
_cell_length_a                   9.676(3)
_cell_length_b                   13.060(3)
_cell_length_c                   13.969(4)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     1681.6(8)
_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      193(2)
_diffrn_measurement_device       'Stoe-Siemens-AED 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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0669
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4941
_diffrn_reflns_theta_max         22.51
_diffrn_reflns_theta_min         2.51
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  90
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.111
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.090
_exptl_crystal_description       blocks
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.027
_refine_ls_goodness_of_fit_obs   1.063
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         4403
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.068
_refine_ls_restrained_S_obs      1.064
_refine_ls_R_factor_all          0.0837
_refine_ls_R_factor_obs          0.0585
_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^)+(0.0801P)^2^+1.1633P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1639
_refine_ls_wR_factor_obs         0.1394
_reflns_number_observed          3297
_reflns_number_total             4406
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9611958_4.cif
_cod_data_source_block           zweig
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0801P)^2^+1.1633P] 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^)+(0.0801P)^2^+1.1633P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4323417