A novel type of formation of zwitterionic compounds, containing two phosphorus atoms of opposite charge and different coordination number
Shevchenko, Igor; Andrushko, Vasyl; Lork, Enno; Röschenthaler, Gerd-Volker; Chemical Communications  (2002) 120–; doi:10.1039/b109484j

data_7114094
_publ_contact_author             'Dr Igor Shevchenko'
_publ_section_title
;
 A novel type of formation of zwitterionic compounds, containing two
 phosphorus atoms of opposite charge and different coordination number
;
_journal_issue                   2
_journal_name_full               'Chemical Communications'
_journal_page_first              120
_journal_paper_doi               10.1039/b109484j
_journal_year                    2002
_chemical_formula_sum            'C19 H36 F7 N3 O P2'
_chemical_formula_weight         517.45
_chemical_melting_point          116.5(15)
_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-97
_cell_angle_alpha                99.440(10)
_cell_angle_beta                 91.68(2)
_cell_angle_gamma                110.99(2)
_cell_formula_units_Z            2
_cell_length_a                   8.987(3)
_cell_length_b                   11.981(3)
_cell_length_c                   12.436(2)
_cell_measurement_reflns_used    38
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.455
_cell_measurement_theta_min      3.322
_cell_volume                     1227.6(6)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_sigmaI/netI    0.0998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4497
_diffrn_reflns_theta_full        23.50
_diffrn_reflns_theta_max         23.50
_diffrn_reflns_theta_min         2.72
_diffrn_standards_decay_%        'random variation +/-2.0'
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.246
_exptl_absorpt_correction_T_max  0.9524
_exptl_absorpt_correction_T_min  0.8662
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.731
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         3605
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.1119
_refine_ls_R_factor_gt           0.0688
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0990P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1560
_refine_ls_wR_factor_ref         0.1748
_reflns_number_gt                2328
_reflns_number_total             3605
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b109484j.txt
_cod_data_source_block           is2a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '115-118' was changed to '116.5(15)'
- the average value was taken and precision was
estimated.

'_symmetry_cell_setting' value 'Triclinic' changed to
'triclinic' according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        1227.6(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7114094