A Tricyclic Phosphorus(V)–Hydrazine System with Twist Conformation of the Central Heterocycle
Engelhardt, Udo; Rosefid, Mehdi; Acta Crystallographica Section C 53 (1997) 773–775; doi:10.1107/S0108270196014898

data_2006199
_publ_section_title
;
 A Tricyclic Phosphorus(V)--Hydrazine System with Twist Conformation of
 the Central Heterocycle
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              773
_journal_page_last               775
_journal_paper_doi               10.1107/S0108270196014898
_journal_volume                  53
_journal_year                    1997
_chemical_formula_sum            'C15 H21 N4 O2 P S'
_chemical_formula_weight         352.14
_chemical_melting_point          385.15
_chemical_name_systematic
; 9-oxo-2-phenoxy-1,3,8,10-tetraaza-2\l^5^-
phosphatricyclo[8.4.0.0^3,8^]tetradecane-2-sulfide
;
_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'
_cell_angle_alpha                90.0
_cell_angle_beta                 91.10(2)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   8.002(5)
_cell_length_b                   12.286(2)
_cell_length_c                   17.380(4)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    293
_cell_measurement_theta_max      14
_cell_measurement_theta_min      7
_cell_volume                     1708.4(12)
_computing_cell_refinement       CAD-4
_computing_data_collection       'CAD-4 (Enraf-Nonius, 1994)'
_computing_data_reduction        CAD-4
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_structure_refinement  'XTAL3.0 (Hall & Stewart, 1990)'
_computing_structure_solution
'MULTAN77 (Main, Lessinger, Woolfson, Germain & Declercq, 1977)'
_diffrn_ambient_temperature      293
_diffrn_measurement_device       'ENRAF-NONIUS CAD4'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.020
_diffrn_reflns_av_sigmaI/netI    0.027
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3241
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         2.5
_diffrn_standards_decay_%        3%
_diffrn_standards_interval_count 100
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.29
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.34
_refine_diff_density_min         -0.29
_refine_ls_extinction_coef       0.29(2)
_refine_ls_extinction_method     'Larson (1967)'
_refine_ls_goodness_of_fit_all   2.48
_refine_ls_goodness_of_fit_obs   2.80
_refine_ls_hydrogen_treatment    'H atoms refined isotropically'
_refine_ls_matrix_type           'full matrix'
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_refine_ls_R_factor_all          0.067
_refine_ls_R_factor_obs          .048
_refine_ls_shift/esd_max         0.017
_refine_ls_shift/esd_mean        0.0029
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/\s^2^(Fo)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.030
_refine_ls_wR_factor_obs         .029
_reflns_number_observed          2378
_reflns_number_total             3008
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            cf1146.cif
_cod_data_source_block           1
_cod_depositor_comments
;
 Changing the _atom_site_aniso_type_symbol data item values from
 'U' to the ones that correspond to the _atom_site_type_symbol data
 item values.

 Antanas Vaitkus,
 2017-01-12

 Adding proper _atom_site_type_symbol data item values instead of
 the placeholder ones ('?').

 Antanas Vaitkus,
 2017-01-12

The following automatic conversions were performed:

'_diffrn_ambient_temperature' value '293 K' was changed to '293' -
the value should be numeric and without a unit
designator.

'_chemical_melting_point' value '112\%C' was changed to
'385.15' - it was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_diffrn_ambient_temperature' value '293 K' was changed to '293' -
the value should be numeric and without a unit
designator.

'_chemical_melting_point' value '112\%C' was changed to
'385.15' - it was converted from degrees Celsius(C) to
Kelvins(K).

'_geom_torsion_publ_flag' value 'Y' changed to 'y'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (6
times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/\s^2^(Fo)' 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)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1708.0(10)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2006199