Phosphorus-nitrogen compounds. Part 13. Syntheses, crystal structures, spectroscopic, stereogenic, and anisochronic properties of novel spiro-ansa-spiro-, spiro-bino-spiro-, and spiro-crypta phosphazene derivatives.
Bilge, Selen; Demiriz, Semsay; Okumus, Aytug; Kiliç, Zeynel; Tercan, Baris; Hökelek, Tuncer; Büyükgüngör, Orhan; Inorganic chemistry 45 (2006) 8755–8767; doi:10.1021/ic060630n

data_4350332
_publ_section_title
;
 Phosphorus-nitrogen compounds. Part 13. Syntheses, crystal structures,
 spectroscopic, stereogenic, and anisochronic properties of novel
 spiro-ansa-spiro-, spiro-bino-spiro-, and spiro-crypta phosphazene
 derivatives.
;
_journal_issue                   21
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8755
_journal_page_last               8767
_journal_paper_doi               10.1021/ic060630n
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C19 H22 Cl4 N5 O2 P3'
_chemical_formula_sum            'C19 H22 Cl4 N5 O2 P3'
_chemical_formula_weight         587.13
_chemical_name_systematic
;
"7,11-(Etane-1,2-diyldioxydi-o-phenylene-dimethylene)-4,4,6,6-
tetrachloro-2(lambda)**5, 4(lambda)**5,6(lambda)**5-triphosphaza(6-P**V)-
1,3,5,7,11-pentaaza-spiro[5.5]dodeca-1,3,5-triene "

by

"Selen Bilge,  &#x00DE;emsay Demiriz,  Aytu&#x00F0; Okumu&#x00FE;,  Zeynel K&#x00FD;l&#x00FD;&#x00E7;, 
Bar&#x00FD;&#x00FE; Tercan, Tuncer H&#x00F6;kelek, Orhan B&#x00FC;y&#x00FC;kg&#x00FC;ng&#x00F6;r"  
;
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   8.5470(3)
_cell_length_b                   21.8940(11)
_cell_length_c                   26.3773(10)
_cell_measurement_reflns_used    2428
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.14
_cell_measurement_theta_min      1.80
_cell_volume                     4935.9(4)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)''
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0826
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            29107
_diffrn_reflns_theta_full        26.04
_diffrn_reflns_theta_max         26.04
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.703
_exptl_absorpt_correction_T_max  0.9204
_exptl_absorpt_correction_T_min  0.7663
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED (Stoe & Cie, 2002)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         4830
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.937
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0377P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0679
_reflns_number_gt                3745
_reflns_number_total             4830
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic060630nsi20060413_051147.cif
_cod_data_source_block           COMPOUND22
_cod_database_code               4350332