Synthesis, reactivity and structural characterisation of bicyclic tetraphosphapentazanes
Thirupathi, Natesan; Krishnamurthy, Setharampattu S.; Nethaji, Munirathinam; Journal of the Chemical Society, Dalton Transactions  (1998) 1469–; doi:10.1039/a801443d

data_7702306
_publ_section_title
;
 Synthesis, reactivity and structural characterisation of bicyclic
 tetraphosphapentazanes
;
_journal_issue                   9
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1469
_journal_paper_doi               10.1039/a801443d
_journal_year                    1998
_chemical_compound_source        synthesis
_chemical_formula_moiety         (EtN)5P4(O)(OPh)2
_chemical_formula_sum            'C22 H35 N5 O3 P4'
_chemical_formula_weight         541.43
_chemical_melting_point          377.1(10)
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 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                 107.359(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.668(2)
_cell_length_b                   34.879(7)
_cell_length_c                   9.7837(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      8
_cell_volume                     2823.2(9)
_computing_cell_refinement       'least-square refinement'
_computing_data_collection       'Enraf-Nonius CAD-4 Program'
_computing_data_reduction        local
_computing_molecular_graphics    'ORTEP II'
_computing_publication_material  CIF
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      290(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4 diffractometer'
_diffrn_measurement_method       'w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0711
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5299
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.17
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  '3600 sec'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.299
_exptl_absorpt_correction_type   'not applied'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         .459
_refine_diff_density_min         -.237
_refine_diff_density_rms         .058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.105
_refine_ls_goodness_of_fit_obs   1.175
_refine_ls_hydrogen_treatment    constraint
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         4949
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.124
_refine_ls_restrained_S_obs      1.201
_refine_ls_R_factor_all          0.1625
_refine_ls_R_factor_obs          0.0765
_refine_ls_shift/esd_max         -0.077
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.0743P)^2^+3.7833P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2185
_refine_ls_wR_factor_obs         0.1616
_reflns_number_observed          2530
_reflns_number_total             4954
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            d801443.txt
_cod_data_source_block           bicy
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '103-105 deg' was changed
to '377.1(10)' -- it was converted from degrees Celsius(C) to
Kelvins(K), the average value was taken and precision was estimated.

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

data item '_refine_ls_weighting_scheme' value 'calc
w=1/[s^2^(Fo^2^)+( 0.0743P)^2^+3.7833P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. A new data item '_refine_ls_weighting_details' was
created with the value set to 'w=1/[s^2^(Fo^2^)+(
0.0743P)^2^+3.7833P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7702306