#------------------------------------------------------------------------------
#$Date: 2017-10-13 14:42:48 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201982 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/04/4310429.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4310429
loop_
_publ_author_name
'Eric Rivard'
'Alan J. Lough'
'Tristram Chivers'
'Ian Manners'
_publ_section_title
;
 Synthesis of Linear and Cyclic Carbophosphazenes via an Oxidative
 Chlorination Strategy
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              802
_journal_page_last               811
_journal_paper_doi               10.1021/ic034954c
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'C25 H33 N2 P Si2'
_chemical_formula_sum            'C25 H33 N2 P Si2'
_chemical_formula_weight         448.68
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.5890(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.0491(3)
_cell_length_b                   11.6549(3)
_cell_length_c                   17.0704(4)
_cell_measurement_reflns_used    5788
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.55
_cell_volume                     2579.02(11)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2002)'
_computing_data_reduction        Denzo-SMN
_computing_molecular_graphics    'SHELXTL V6.12'
_computing_publication_material  'SHELXTL V6.12'
_computing_structure_refinement  'SHELXTL V6.12(Sheldrick, 2001)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'φ scans and ω scans with κ offsets'
_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  0.074
_diffrn_reflns_av_sigmaI/netI    0.0744
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19724
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.72
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.214
_exptl_absorpt_correction_T_max  0.9790
_exptl_absorpt_correction_T_min  0.9505
_exptl_absorpt_correction_type   mutli-scan
_exptl_absorpt_process_details   'Denzo-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       0.0031(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         5898
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0485
_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/[σ²(Fo²)+(0.0621P)²+0.5132P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1338
_reflns_number_gt                4088
_reflns_number_total             5898
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic034954csi20031103_051734_1.cif
_cod_data_source_block           compound(1)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4310429
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.03657(4) 0.90164(5) 0.18181(3) 0.02240(15) Uani 1 1 d . . .
Si1 Si 0.35396(4) 0.84001(6) 0.27129(3) 0.02746(17) Uani 1 1 d . . .
Si2 Si 0.27941(5) 0.99189(6) 0.12504(4) 0.03166(18) Uani 1 1 d . . .
N1 N 0.10169(12) 0.78469(16) 0.14990(9) 0.0230(4) Uani 1 1 d . . .
N2 N 0.27003(12) 0.86903(16) 0.18464(9) 0.0237(4) Uani 1 1 d . . .
C1 C 0.20008(15) 0.78073(18) 0.15534(10) 0.0217(4) Uani 1 1 d . . .
C2 C 0.24638(16) 0.67239(19) 0.12856(11) 0.0262(5) Uani 1 1 d . . .
C3 C 0.19632(18) 0.5682(2) 0.13682(12) 0.0329(5) Uani 1 1 d . . .
H3A H 0.1325 0.5666 0.1586 0.039 Uiso 1 1 calc R . .
C4 C 0.2393(2) 0.4671(2) 0.11341(15) 0.0470(7) Uani 1 1 d . . .
H4A H 0.2057 0.3960 0.1202 0.056 Uiso 1 1 calc R . .
C5 C 0.3305(2) 0.4692(3) 0.08027(15) 0.0504(8) Uani 1 1 d . . .
H5A H 0.3602 0.3995 0.0649 0.061 Uiso 1 1 calc R . .
C6 C 0.3789(2) 0.5718(3) 0.06938(15) 0.0450(7) Uani 1 1 d . . .
H6A H 0.4405 0.5731 0.0447 0.054 Uiso 1 1 calc R . .
C7 C 0.33794(17) 0.6733(2) 0.09429(13) 0.0353(6) Uani 1 1 d . . .
H7A H 0.3726 0.7438 0.0879 0.042 Uiso 1 1 calc R . .
C8 C 0.48445(18) 0.7893(3) 0.25251(16) 0.0469(7) Uani 1 1 d . . .
H8A H 0.5168 0.8470 0.2216 0.070 Uiso 1 1 calc R . .
H8B H 0.4779 0.7169 0.2232 0.070 Uiso 1 1 calc R . .
H8C H 0.5272 0.7773 0.3029 0.070 Uiso 1 1 calc R . .
C9 C 0.3710(2) 0.9740(2) 0.32972(15) 0.0435(6) Uani 1 1 d . . .
H9A H 0.3034 1.0025 0.3407 0.065 Uiso 1 1 calc R . .
H9B H 0.4046 1.0320 0.2998 0.065 Uiso 1 1 calc R . .
H9C H 0.4139 0.9586 0.3795 0.065 Uiso 1 1 calc R . .
C10 C 0.29715(19) 0.7278(2) 0.32961(14) 0.0411(6) Uani 1 1 d . . .
H10A H 0.2283 0.7519 0.3407 0.062 Uiso 1 1 calc R . .
H10B H 0.3413 0.7161 0.3794 0.062 Uiso 1 1 calc R . .
H10C H 0.2917 0.6559 0.2997 0.062 Uiso 1 1 calc R . .
C11 C 0.4165(2) 1.0100(3) 0.10513(18) 0.0504(7) Uani 1 1 d . . .
H11A H 0.4603 1.0227 0.1550 0.076 Uiso 1 1 calc R . .
H11B H 0.4217 1.0762 0.0704 0.076 Uiso 1 1 calc R . .
H11C H 0.4393 0.9407 0.0796 0.076 Uiso 1 1 calc R . .
C12 C 0.24265(19) 1.1269(2) 0.17147(16) 0.0427(6) Uani 1 1 d . . .
H12A H 0.1709 1.1217 0.1829 0.064 Uiso 1 1 calc R . .
H12B H 0.2497 1.1911 0.1354 0.064 Uiso 1 1 calc R . .
H12C H 0.2879 1.1394 0.2206 0.064 Uiso 1 1 calc R . .
C13 C 0.1982(2) 0.9682(2) 0.02957(14) 0.0451(7) Uani 1 1 d . . .
H13A H 0.1260 0.9591 0.0391 0.068 Uiso 1 1 calc R . .
H13B H 0.2213 0.8988 0.0044 0.068 Uiso 1 1 calc R . .
H13C H 0.2044 1.0343 -0.0050 0.068 Uiso 1 1 calc R . .
C14 C 0.04381(15) 0.8693(2) 0.28746(11) 0.0245(5) Uani 1 1 d . . .
C15 C 0.01663(17) 0.7624(2) 0.31480(12) 0.0321(5) Uani 1 1 d . . .
H15A H -0.0079 0.7045 0.2782 0.039 Uiso 1 1 calc R . .
C16 C 0.02511(18) 0.7397(2) 0.39529(13) 0.0369(6) Uani 1 1 d . . .
H16A H 0.0067 0.6663 0.4135 0.044 Uiso 1 1 calc R . .
C17 C 0.06038(17) 0.8240(2) 0.44898(13) 0.0370(6) Uani 1 1 d . . .
H17A H 0.0667 0.8084 0.5039 0.044 Uiso 1 1 calc R . .
C18 C 0.08628(18) 0.9306(2) 0.42232(13) 0.0376(6) Uani 1 1 d . . .
H18A H 0.1095 0.9889 0.4591 0.045 Uiso 1 1 calc R . .
C19 C 0.07863(17) 0.9535(2) 0.34165(12) 0.0299(5) Uani 1 1 d . . .
H19A H 0.0973 1.0269 0.3237 0.036 Uiso 1 1 calc R . .
C20 C -0.09567(15) 0.85312(18) 0.15136(11) 0.0224(4) Uani 1 1 d . . .
C21 C -0.12135(17) 0.7566(2) 0.10613(12) 0.0289(5) Uani 1 1 d . . .
H21A H -0.0683 0.7100 0.0894 0.035 Uiso 1 1 calc R . .
C22 C -0.22430(17) 0.7271(2) 0.08485(13) 0.0355(6) Uani 1 1 d . . .
H22A H -0.2410 0.6608 0.0536 0.043 Uiso 1 1 calc R . .
C23 C -0.30183(17) 0.7938(2) 0.10897(13) 0.0357(6) Uani 1 1 d . . .
H23A H -0.3720 0.7729 0.0953 0.043 Uiso 1 1 calc R . .
C24 C -0.27723(17) 0.8909(2) 0.15310(14) 0.0374(6) Uani 1 1 d . . .
H24A H -0.3306 0.9376 0.1694 0.045 Uiso 1 1 calc R . .
C25 C -0.17520(16) 0.9209(2) 0.17374(13) 0.0318(5) Uani 1 1 d . . .
H25A H -0.1591 0.9886 0.2036 0.038 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 P1 C20 98.53(9) . . ?
N1 P1 C14 100.14(9) . . ?
C20 P1 C14 98.97(9) . . ?
N2 Si1 C10 109.72(10) . . ?
N2 Si1 C9 108.26(10) . . ?
C10 Si1 C9 109.70(12) . . ?
N2 Si1 C8 114.00(10) . . ?
C10 Si1 C8 107.37(13) . . ?
C9 Si1 C8 107.73(13) . . ?
N2 Si2 C12 113.81(11) . . ?
N2 Si2 C13 108.30(10) . . ?
C12 Si2 C13 110.60(13) . . ?
N2 Si2 C11 109.06(11) . . ?
C12 Si2 C11 106.39(13) . . ?
C13 Si2 C11 108.55(13) . . ?
C1 N1 P1 122.17(15) . . ?
C1 N2 Si2 117.76(13) . . ?
C1 N2 Si1 117.69(14) . . ?
Si2 N2 Si1 123.96(10) . . ?
N1 C1 N2 126.61(19) . . ?
N1 C1 C2 116.53(18) . . ?
N2 C1 C2 116.86(17) . . ?
C7 C2 C3 119.0(2) . . ?
C7 C2 C1 121.3(2) . . ?
C3 C2 C1 119.66(19) . . ?
C4 C3 C2 120.2(2) . . ?
C5 C4 C3 120.1(3) . . ?
C6 C5 C4 120.2(2) . . ?
C5 C6 C7 120.2(3) . . ?
C6 C7 C2 120.2(2) . . ?
C19 C14 C15 119.08(19) . . ?
C19 C14 P1 119.03(17) . . ?
C15 C14 P1 121.88(16) . . ?
C14 C15 C16 120.5(2) . . ?
C17 C16 C15 120.1(2) . . ?
C18 C17 C16 119.7(2) . . ?
C17 C18 C19 120.4(2) . . ?
C14 C19 C18 120.2(2) . . ?
C21 C20 C25 118.29(19) . . ?
C21 C20 P1 124.66(16) . . ?
C25 C20 P1 117.02(17) . . ?
C20 C21 C22 120.7(2) . . ?
C23 C22 C21 120.2(2) . . ?
C22 C23 C24 119.6(2) . . ?
C23 C24 C25 120.3(2) . . ?
C24 C25 C20 120.9(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 N1 1.7271(18) . ?
P1 C20 1.834(2) . ?
P1 C14 1.834(2) . ?
Si1 N2 1.7691(17) . ?
Si1 C10 1.850(3) . ?
Si1 C9 1.853(3) . ?
Si1 C8 1.865(2) . ?
Si2 N2 1.7689(18) . ?
Si2 C12 1.849(3) . ?
Si2 C13 1.860(2) . ?
Si2 C11 1.871(3) . ?
N1 C1 1.277(3) . ?
N2 C1 1.427(3) . ?
C1 C2 1.494(3) . ?
C2 C7 1.389(3) . ?
C2 C3 1.394(3) . ?
C3 C4 1.384(3) . ?
C4 C5 1.375(4) . ?
C5 C6 1.375(4) . ?
C6 C7 1.384(3) . ?
C14 C19 1.389(3) . ?
C14 C15 1.390(3) . ?
C15 C16 1.391(3) . ?
C16 C17 1.386(4) . ?
C17 C18 1.379(4) . ?
C18 C19 1.395(3) . ?
C20 C21 1.383(3) . ?
C20 C25 1.392(3) . ?
C21 C22 1.394(3) . ?
C22 C23 1.376(3) . ?
C23 C24 1.377(4) . ?
C24 C25 1.382(3) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 4880303
