#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:04:14 +0100 (Fri 25 de Mar de 2016) $
#$Revision: 179774 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/70/7007005.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_7007005
loop_
_publ_author_name
'Prabusankar, Ganesan'
'Palanisami, Nallasamy'
'Murugavel, Ramaswamy'
'Butcher, Ray J.'
_publ_section_title
;
 Sterically encumbered acyclic diphosphazanes: synthesis, conformations
 and coordination behavior.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2140
_journal_page_last               2146
_journal_paper_doi               10.1039/b516316a
_journal_year                    2006
_chemical_formula_sum            'C32 H51 Cl2 N O2 P2'
_chemical_formula_weight         614.58
_chemical_name_systematic
;
?
;
_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                97.828(6)
_cell_angle_beta                 96.701(7)
_cell_angle_gamma                90.327(7)
_cell_formula_units_Z            2
_cell_length_a                   9.3484(10)
_cell_length_b                   12.2160(9)
_cell_length_c                   15.4244(11)
_cell_measurement_temperature    293(2)
_cell_volume                     1732.7(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0096
_diffrn_reflns_av_sigmaI/netI    0.0226
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6502
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    0.307
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             660
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         6088
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0712
_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)+(0.0458P)²+1.4769P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1207
_refine_ls_wR_factor_ref         0.1311
_reflns_number_gt                4695
_reflns_number_total             6088
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b516316a.txt
_cod_data_source_block           rm102a
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7007005
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.80503(8) 0.29839(7) 0.08216(4) 0.0515(2) Uani 1 1 d . . .
P2 P 0.76623(8) 0.19806(7) -0.09022(5) 0.0512(2) Uani 1 1 d . . .
N1 N 0.8879(2) 0.2480(3) -0.00505(15) 0.0661(8) Uani 1 1 d . . .
O1 O 0.89420(18) 0.23822(15) 0.15938(11) 0.0456(4) Uani 1 1 d . . .
O2 O 0.82024(18) 0.26129(15) -0.16792(11) 0.0448(4) Uani 1 1 d . . .
Cl1 Cl 0.89595(11) 0.45828(8) 0.11260(6) 0.0787(3) Uani 1 1 d . . .
Cl2 Cl 0.84389(12) 0.04001(8) -0.12537(6) 0.0814(3) Uani 1 1 d . . .
C1 C 0.8356(3) 0.2570(2) 0.24095(15) 0.0405(6) Uani 1 1 d . . .
C2 C 0.7013(3) 0.2085(2) 0.24787(17) 0.0453(6) Uani 1 1 d . . .
C3 C 0.6337(3) 0.2524(3) 0.32080(18) 0.0538(7) Uani 1 1 d . . .
H3 H 0.5422 0.2256 0.3259 0.065 Uiso 1 1 calc R . .
C4 C 0.6957(3) 0.3332(3) 0.38539(18) 0.0542(7) Uani 1 1 d . . .
C5 C 0.8363(3) 0.3646(2) 0.38117(17) 0.0524(7) Uani 1 1 d . . .
H5 H 0.8825 0.4134 0.4277 0.063 Uiso 1 1 calc R . .
C6 C 0.9132(3) 0.3272(2) 0.31081(16) 0.0427(6) Uani 1 1 d . . .
C7 C 0.6251(3) 0.1086(2) 0.18656(19) 0.0559(7) Uani 1 1 d . . .
C8 C 0.4944(4) 0.1473(3) 0.1292(2) 0.0812(11) Uani 1 1 d . . .
H8A H 0.5264 0.1972 0.0921 0.122 Uiso 1 1 calc R . .
H8B H 0.4292 0.1843 0.1665 0.122 Uiso 1 1 calc R . .
H8C H 0.4462 0.0844 0.0933 0.122 Uiso 1 1 calc R . .
C9 C 0.5726(5) 0.0270(3) 0.2442(3) 0.0904(12) Uani 1 1 d . . .
H9A H 0.6514 0.0096 0.2854 0.136 Uiso 1 1 calc R . .
H9B H 0.5361 -0.0394 0.2074 0.136 Uiso 1 1 calc R . .
H9C H 0.4974 0.0600 0.2757 0.136 Uiso 1 1 calc R . .
C10 C 0.7228(4) 0.0419(3) 0.1261(3) 0.0797(10) Uani 1 1 d . . .
H10A H 0.7391 0.0822 0.0788 0.119 Uiso 1 1 calc R . .
H10B H 0.6770 -0.0281 0.1024 0.119 Uiso 1 1 calc R . .
H10C H 0.8133 0.0299 0.1595 0.119 Uiso 1 1 calc R . .
C11 C 0.6150(4) 0.3840(3) 0.4597(2) 0.0803(11) Uani 1 1 d . . .
H11A H 0.5207 0.3503 0.4535 0.120 Uiso 1 1 calc R . .
H11B H 0.6064 0.4619 0.4578 0.120 Uiso 1 1 calc R . .
H11C H 0.6666 0.3721 0.5150 0.120 Uiso 1 1 calc R . .
C12 C 1.0745(3) 0.3604(2) 0.32122(17) 0.0494(6) Uani 1 1 d . . .
C13 C 1.0934(4) 0.4868(3) 0.3306(2) 0.0698(9) Uani 1 1 d . . .
H13A H 1.1942 0.5064 0.3414 0.105 Uiso 1 1 calc R . .
H13B H 1.0456 0.5203 0.3790 0.105 Uiso 1 1 calc R . .
H13C H 1.0523 0.5125 0.2772 0.105 Uiso 1 1 calc R . .
C14 C 1.1438(3) 0.3211(3) 0.4072(2) 0.0715(9) Uani 1 1 d . . .
H14A H 1.2446 0.3405 0.4164 0.107 Uiso 1 1 calc R . .
H14B H 1.1319 0.2423 0.4028 0.107 Uiso 1 1 calc R . .
H14C H 1.0979 0.3560 0.4560 0.107 Uiso 1 1 calc R . .
C15 C 1.1598(3) 0.3082(3) 0.2481(2) 0.0619(8) Uani 1 1 d . . .
H15A H 1.2605 0.3253 0.2645 0.093 Uiso 1 1 calc R . .
H15B H 1.1278 0.3369 0.1944 0.093 Uiso 1 1 calc R . .
H15C H 1.1447 0.2294 0.2395 0.093 Uiso 1 1 calc R . .
C16 C 0.7243(3) 0.2471(2) -0.24706(15) 0.0406(6) Uani 1 1 d . . .
C17 C 0.7674(3) 0.1814(2) -0.32117(16) 0.0453(6) Uani 1 1 d . . .
C18 C 0.6584(3) 0.1501(2) -0.38998(18) 0.0558(7) Uani 1 1 d . . .
H18 H 0.6819 0.1044 -0.4394 0.067 Uiso 1 1 calc R . .
C19 C 0.5181(3) 0.1830(3) -0.38877(19) 0.0574(7) Uani 1 1 d . . .
C20 C 0.4875(3) 0.2592(3) -0.31967(19) 0.0555(7) Uani 1 1 d . . .
H20 H 0.3949 0.2868 -0.3208 0.067 Uiso 1 1 calc R . .
C21 C 0.5887(3) 0.2972(2) -0.24780(17) 0.0451(6) Uani 1 1 d . . .
C22 C 0.9217(3) 0.1460(2) -0.33769(18) 0.0519(7) Uani 1 1 d . . .
C23 C 1.0422(3) 0.1929(3) -0.2661(2) 0.0617(8) Uani 1 1 d . . .
H23A H 1.1340 0.1757 -0.2860 0.093 Uiso 1 1 calc R . .
H23B H 1.0342 0.1608 -0.2133 0.093 Uiso 1 1 calc R . .
H23C H 1.0339 0.2716 -0.2540 0.093 Uiso 1 1 calc R . .
C24 C 0.9540(4) 0.1892(3) -0.4232(2) 0.0768(10) Uani 1 1 d . . .
H24A H 0.8853 0.1576 -0.4714 0.115 Uiso 1 1 calc R . .
H24B H 1.0494 0.1687 -0.4354 0.115 Uiso 1 1 calc R . .
H24C H 0.9475 0.2683 -0.4160 0.115 Uiso 1 1 calc R . .
C25 C 0.9300(4) 0.0190(3) -0.3512(2) 0.0757(10) Uani 1 1 d . . .
H25A H 0.8601 -0.0111 -0.3992 0.114 Uiso 1 1 calc R . .
H25B H 0.9105 -0.0088 -0.2984 0.114 Uiso 1 1 calc R . .
H25C H 1.0247 -0.0021 -0.3644 0.114 Uiso 1 1 calc R . .
C26 C 0.4016(4) 0.1402(3) -0.4628(2) 0.0872(12) Uani 1 1 d . . .
H26A H 0.4436 0.1235 -0.5168 0.131 Uiso 1 1 calc R . .
H26B H 0.3300 0.1955 -0.4691 0.131 Uiso 1 1 calc R . .
H26C H 0.3574 0.0744 -0.4492 0.131 Uiso 1 1 calc R . .
C27 C 0.5427(3) 0.3929(2) -0.18081(19) 0.0550(7) Uani 1 1 d . . .
C28 C 0.4678(4) 0.4800(3) -0.2333(3) 0.0828(11) Uani 1 1 d . . .
H28A H 0.3791 0.4492 -0.2652 0.124 Uiso 1 1 calc R . .
H28B H 0.5297 0.5010 -0.2739 0.124 Uiso 1 1 calc R . .
H28C H 0.4479 0.5439 -0.1932 0.124 Uiso 1 1 calc R . .
C29 C 0.6667(4) 0.4557(3) -0.1201(2) 0.0713(9) Uani 1 1 d . . .
H29A H 0.7430 0.4697 -0.1540 0.107 Uiso 1 1 calc R . .
H29B H 0.7020 0.4120 -0.0752 0.107 Uiso 1 1 calc R . .
H29C H 0.6327 0.5246 -0.0931 0.107 Uiso 1 1 calc R . .
C30 C 0.4342(4) 0.3492(3) -0.1247(2) 0.0819(11) Uani 1 1 d . . .
H30A H 0.3542 0.3132 -0.1628 0.123 Uiso 1 1 calc R . .
H30B H 0.4003 0.4099 -0.0867 0.123 Uiso 1 1 calc R . .
H30C H 0.4808 0.2975 -0.0897 0.123 Uiso 1 1 calc R . .
C31 C 1.0723(8) 0.2875(4) -0.0177(3) 0.143(3) Uani 1 1 d . . .
H31A H 1.0894 0.2916 -0.0780 0.172 Uiso 1 1 calc R . .
H31B H 1.1104 0.3524 0.0217 0.172 Uiso 1 1 calc R . .
C32 C 1.1047(9) 0.1979(4) 0.0088(3) 0.173(3) Uani 1 1 d . . .
H32A H 1.0885 0.2014 0.0694 0.260 Uiso 1 1 calc R . .
H32B H 1.2045 0.1839 0.0034 0.260 Uiso 1 1 calc R . .
H32C H 1.0462 0.1394 -0.0261 0.260 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'
O O 0.0106 0.0060 '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'
Cl Cl 0.1484 0.1585 '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
O1 P1 N1 100.72(11) . . ?
O1 P1 Cl1 100.22(8) . . ?
N1 P1 Cl1 101.36(11) . . ?
O2 P2 N1 100.34(12) . . ?
O2 P2 Cl2 100.05(8) . . ?
N1 P2 Cl2 101.57(11) . . ?
P1 N1 P2 110.35(13) . . ?
P1 N1 C31 123.0(2) . . ?
P2 N1 C31 123.23(19) . . ?
C1 O1 P1 113.15(15) . . ?
C16 O2 P2 113.57(15) . . ?
C2 C1 C6 122.8(2) . . ?
C2 C1 O1 119.2(2) . . ?
C6 C1 O1 118.0(2) . . ?
C3 C2 C1 115.7(2) . . ?
C3 C2 C7 117.1(2) . . ?
C1 C2 C7 127.1(2) . . ?
C4 C3 C2 123.4(3) . . ?
C3 C4 C5 117.5(2) . . ?
C3 C4 C11 121.7(3) . . ?
C5 C4 C11 120.8(3) . . ?
C4 C5 C6 123.6(3) . . ?
C5 C6 C1 115.5(2) . . ?
C5 C6 C12 116.9(2) . . ?
C1 C6 C12 127.5(2) . . ?
C9 C7 C8 108.9(3) . . ?
C9 C7 C10 105.7(3) . . ?
C8 C7 C10 108.7(3) . . ?
C9 C7 C2 108.5(3) . . ?
C8 C7 C2 110.3(3) . . ?
C10 C7 C2 114.5(2) . . ?
C15 C12 C13 108.7(3) . . ?
C15 C12 C6 115.8(2) . . ?
C13 C12 C6 110.5(2) . . ?
C15 C12 C14 106.4(2) . . ?
C13 C12 C14 108.4(2) . . ?
C6 C12 C14 106.8(2) . . ?
C17 C16 C21 122.7(2) . . ?
C17 C16 O2 118.4(2) . . ?
C21 C16 O2 118.9(2) . . ?
C18 C17 C16 115.5(2) . . ?
C18 C17 C22 116.4(2) . . ?
C16 C17 C22 127.9(2) . . ?
C19 C18 C17 123.6(3) . . ?
C20 C19 C18 117.8(3) . . ?
C20 C19 C26 120.8(3) . . ?
C18 C19 C26 121.4(3) . . ?
C19 C20 C21 123.2(3) . . ?
C20 C21 C16 115.7(2) . . ?
C20 C21 C27 116.8(2) . . ?
C16 C21 C27 127.4(2) . . ?
C23 C22 C25 108.7(3) . . ?
C23 C22 C24 106.2(3) . . ?
C25 C22 C24 108.7(3) . . ?
C23 C22 C17 115.6(2) . . ?
C25 C22 C17 110.1(3) . . ?
C24 C22 C17 107.3(2) . . ?
C29 C27 C28 105.3(3) . . ?
C29 C27 C30 109.6(3) . . ?
C28 C27 C30 108.6(3) . . ?
C29 C27 C21 115.2(2) . . ?
C28 C27 C21 108.0(2) . . ?
C30 C27 C21 109.9(3) . . ?
C32 C31 N1 84.8(5) . . ?
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 O1 1.6333(18) . ?
P1 N1 1.677(2) . ?
P1 Cl1 2.0966(13) . ?
P2 O2 1.6361(19) . ?
P2 N1 1.678(2) . ?
P2 Cl2 2.0908(13) . ?
N1 C31 1.826(7) . ?
O1 C1 1.421(3) . ?
O2 C16 1.418(3) . ?
C1 C2 1.406(4) . ?
C1 C6 1.408(3) . ?
C2 C3 1.399(4) . ?
C2 C7 1.553(4) . ?
C3 C4 1.376(4) . ?
C4 C5 1.378(4) . ?
C4 C11 1.510(4) . ?
C5 C6 1.398(4) . ?
C6 C12 1.544(4) . ?
C7 C9 1.536(5) . ?
C7 C8 1.538(4) . ?
C7 C10 1.539(4) . ?
C12 C15 1.528(4) . ?
C12 C13 1.538(4) . ?
C12 C14 1.545(4) . ?
C16 C17 1.405(3) . ?
C16 C21 1.409(4) . ?
C17 C18 1.394(4) . ?
C17 C22 1.548(4) . ?
C18 C19 1.376(4) . ?
C19 C20 1.374(4) . ?
C19 C26 1.518(4) . ?
C20 C21 1.397(4) . ?
C21 C27 1.550(4) . ?
C22 C23 1.532(4) . ?
C22 C25 1.540(4) . ?
C22 C24 1.547(4) . ?
C27 C29 1.533(4) . ?
C27 C28 1.545(4) . ?
C27 C30 1.545(4) . ?
C31 C32 1.246(6) . ?
