2,2-[2,2'-Methylenebis(4-nitrophenoxy)]-4,6-[2,2'-methylenebis(4-nitrophenoxy)]-4,6-dichloro-1,3,5,2λ^5^,4λ^5^,6λ^5^-triazatriphosphorine (spiro-ansa) acetonitrile
Öztürk, Levent; Hökelek, Tuncer; Dal, Hakan; Kılıç, Zeynel; Acta Crystallographica Section E 58 (2002) o20–o23; doi:10.1107/S1600536801020463

data_2200981
_publ_section_title
;2,2-[2,2'-Methylenebis(4-nitrophenoxy)]-4,6-[2,2'-methylenebis(4-nitrophenoxy)]-4,6-dichloro-1,3,5,2\l^5^,4\l^5^,6\l^5^-triazatriphosphorine
 (spiro-ansa) acetonitrile
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o20
_journal_page_last               o23
_journal_paper_doi               10.1107/S1600536801020463
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          'C26 H16 Cl2 N7 O12 P3, C2 H3 N'
_chemical_formula_moiety         'C26 H16 Cl2 N7 O12 P3, C2 H3 N'
_chemical_formula_sum            'C28 H19 Cl2 N8 O12 P3'
_chemical_formula_weight         823.32
_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                97.493(10)
_cell_angle_beta                 109.989(10)
_cell_angle_gamma                109.776(10)
_cell_formula_units_Z            2
_cell_length_a                   11.5487(10)
_cell_length_b                   11.8570(10)
_cell_length_c                   15.0238(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      42
_cell_measurement_theta_min      16
_cell_volume                     1747.5(3)
_computing_cell_refinement       'CAD-4 EXPRESS'
_computing_data_collection       'CAD-4 EXPRESS (Enraf-Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX  (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       'non-profiled \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Cuk\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  .0341
_diffrn_reflns_av_sigmaI/netI    .0479
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7549
_diffrn_reflns_theta_full        74.24
_diffrn_reflns_theta_max         74.24
_diffrn_reflns_theta_min         4.67
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.626
_exptl_absorpt_correction_T_max  .484
_exptl_absorpt_correction_T_min  .388
_exptl_absorpt_correction_type   '\y scans'
_exptl_absorpt_process_details   '(MolEN; Fair, 1990)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block-like
_exptl_crystal_F_000             836
_exptl_crystal_size_max          .30
_exptl_crystal_size_mid          .25
_exptl_crystal_size_min          .20
_refine_diff_density_max         1.100
_refine_diff_density_min         -.556
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         6411
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          .0991
_refine_ls_R_factor_gt           .0667
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.1313p)^2^] where p = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          .1695
_refine_ls_wR_factor_ref         .1939
_reflns_number_gt                4690
_reflns_number_total             7127
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wn6072.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_adp_type' value 'uani' changed to 'Uani' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (53
times).

'_atom_site_adp_type' value 'uiso' changed to 'Uiso' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (19
times).

'_atom_site_calc_flag' value 'Calc' changed to 'calc' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_atom_site_refinement_flags' value 'r' changed to 'R'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (19 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_atom_site_adp_type' value 'uani' changed to 'Uani' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (53
times).

'_atom_site_adp_type' value 'uiso' changed to 'Uiso'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (19
times).

'_atom_site_calc_flag' value 'Calc' changed to 'calc'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_atom_site_refinement_flags' value 'r' changed to 'R'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (19
times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1747.5(2)
_cod_database_code               2200981
_cod_database_fobs_code          2200981