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_4323414
_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            'C43 H63 N O4.5 P'
_chemical_formula_weight         696.91
_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                 95.930(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4990(10)
_cell_length_b                   18.9710(10)
_cell_length_c                   23.478(2)
_cell_measurement_reflns_used    48
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     4208.2(6)
_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-difractometer'
_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  0.0599
_diffrn_reflns_av_sigmaI/netI    0.0513
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            9259
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         3.56
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  90
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.105
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.100
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1516
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         .669
_refine_diff_density_min         -.406
_refine_diff_density_rms         .059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.028
_refine_ls_goodness_of_fit_obs   1.068
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         7453
_refine_ls_number_restraints     240
_refine_ls_restrained_S_all      1.060
_refine_ls_restrained_S_obs      1.093
_refine_ls_R_factor_all          0.0940
_refine_ls_R_factor_obs          0.0634
_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^)+( 0.0920P)^2^+3.2199P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1864
_refine_ls_wR_factor_obs         0.1596
_reflns_number_observed          5306
_reflns_number_total             7458
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9611958_1.cif
_cod_data_source_block           kck30
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0920P)^2^+3.2199P] 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^)+( 0.0920P)^2^+3.2199P] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C43 H63 N O4.50 P'
_cod_database_code               4323414