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_4350331
_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         'C30 H40 N7 O6 P3'
_chemical_formula_sum            'C30 H40 N7 O6 P3'
_chemical_formula_weight         687.60
_chemical_name_systematic
;
"18,19-Dihydro-8,8-bis(1,4-dioxa-8-azaspiro[4,5]decane)-1-yl-
6(lambda)**5,8(lambda)**5,10(lambda)**5-6,10-nit-rilo-16H,21H-
[1,3,5,7,2,4,6]tetrazatriphosphonino[2,1-b:6,7-b']bis[1,3,2]benzoxaza-
phosphorine "

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           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_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                 99.243(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.4420(11)
_cell_length_b                   13.3370(9)
_cell_length_c                   13.5691(14)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.6
_cell_measurement_theta_min      3.2
_cell_volume                     3294.1(5)
_computing_cell_refinement       'CAD4 Express'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_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      296(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_method       'non-profiled omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0294
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3395
_diffrn_reflns_theta_full        74.25
_diffrn_reflns_theta_max         74.25
_diffrn_reflns_theta_min         4.11
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.113
_exptl_absorpt_correction_T_max  0.589
_exptl_absorpt_correction_T_min  0.499
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
Number of psi-scan sets used was   5
Theta correction was applied.
Averaged transmission function was used.
No Fourier smoothing was applied.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.941
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.117
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.08(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         3395
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0592
_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^)+(0.1033P)^2^+0.3520P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1394
_refine_ls_wR_factor_ref         0.1469
_reflns_number_gt                3077
_reflns_number_total             3395
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic060630nsi20060413_051147.cif
_cod_data_source_block           COMPOUND16
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4350331