#------------------------------------------------------------------------------
#$Date: 2016-02-05 01:51:25 +0200 (Fri, 05 Feb 2016) $
#$Revision: 176064 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/75/7037519.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_7037519
loop_
_publ_author_name
'Sevilla, Raquel'
'Less, Robert J.'
'García-Rodríguez, Raúl'
'Bond, Andrew D.'
'Wright, Dominic S.'
_publ_section_title
;
 Synthesis and structure of the extended phosphazane ligand
 [(1,4-C6H4){N(μ-PN(t)Bu)2N(t)Bu}2](4.).
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1868
_journal_page_last               1871
_journal_paper_doi               10.1039/c5dt04393j
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C30 H62 N8 P4'
_chemical_formula_sum            'C30 H62 N8 P4'
_chemical_formula_weight         658.75
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-11-04 deposited with the CCDC.
2015-12-02 downloaded from the CCDC.
;
_cell_angle_alpha                106.920(4)
_cell_angle_beta                 98.179(6)
_cell_angle_gamma                100.308(10)
_cell_formula_units_Z            1
_cell_length_a                   6.0734(9)
_cell_length_b                   12.3908(14)
_cell_length_c                   14.032(2)
_cell_measurement_reflns_used    29918
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      22.46
_cell_measurement_theta_min      1.00
_cell_volume                     972.5(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  SHELXL
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω and φ-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_laue_measured_fraction_full 0.951
_diffrn_reflns_laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4947
_diffrn_reflns_point_group_measured_fraction_full 0.951
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        22.442
_diffrn_reflns_theta_max         22.442
_diffrn_reflns_theta_min         3.521
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.224
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_description       block
_exptl_crystal_F_000             358
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.282
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2396
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.281
_refine_ls_R_factor_all          0.0963
_refine_ls_R_factor_gt           0.0831
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+3.2317P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1882
_refine_ls_wR_factor_ref         0.1937
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2051
_reflns_number_total             2396
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5dt04393j2.cif
_cod_data_source_block           1H4
_cod_depositor_comments
'Adding full bibliography for 7037519--7037522.cif.'
_cod_database_code               7037519
_cambridge_user_name             'Raquel Sevilla-Martin'
_cambridge_user_crsid            rs617
_cambridge_supervisor_name       'Dominic Wright'
_cambridge_supervisor_crsid      dsw1000
_cambridge_crystallographer_name 'Andrew Bond'
_cambridge_crystallographer_crsid adb29
_cambridge_sample_id             RSM74C
_cambridge_data_id               dw_k3_0007
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.969
_shelx_estimated_absorpt_t_max   0.974
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
P1 P 0.5677(3) 0.43135(15) 0.23201(13) 0.0330(5) Uani 1 1 d . .
P2 P 0.5654(3) 0.23113(15) 0.26259(13) 0.0343(5) Uani 1 1 d . .
N1 N 0.3439(12) 0.1754(6) 0.3040(5) 0.0521(17) Uani 1 1 d D .
H1 H 0.234(10) 0.212(6) 0.298(6) 0.07(3) Uiso 1 1 d D .
N2 N 0.3532(10) 0.4936(5) 0.2555(5) 0.0393(14) Uani 1 1 d D .
H2 H 0.224(6) 0.450(5) 0.258(5) 0.04(2) Uiso 1 1 d D .
N3 N 0.4442(9) 0.2849(4) 0.1719(4) 0.0317(13) Uani 1 1 d . .
N4 N 0.6343(10) 0.3772(4) 0.3310(4) 0.0358(14) Uani 1 1 d . .
C1 C 0.2940(13) 0.0699(6) 0.3322(5) 0.0429(18) Uani 1 1 d . .
C11 C 0.1075(18) -0.0229(8) 0.2509(6) 0.081(3) Uani 1 1 d . .
H11A H 0.0637 -0.0892 0.2745 0.121 Uiso 1 1 calc R U
H11B H 0.1646 -0.0483 0.1881 0.121 Uiso 1 1 calc R U
H11C H -0.0260 0.0088 0.2377 0.121 Uiso 1 1 calc R U
C12 C 0.2081(17) 0.1000(7) 0.4314(6) 0.068(3) Uani 1 1 d . .
H12A H 0.1652 0.0296 0.4495 0.103 Uiso 1 1 calc R U
H12B H 0.0744 0.1330 0.4227 0.103 Uiso 1 1 calc R U
H12C H 0.3294 0.1567 0.4857 0.103 Uiso 1 1 calc R U
C13 C 0.5076(15) 0.0257(8) 0.3480(8) 0.077(3) Uani 1 1 d . .
H13A H 0.4748 -0.0409 0.3722 0.115 Uiso 1 1 calc R U
H13B H 0.6282 0.0874 0.3986 0.115 Uiso 1 1 calc R U
H13C H 0.5586 0.0019 0.2835 0.115 Uiso 1 1 calc R U
C2 C 0.3265(12) 0.6073(6) 0.2510(5) 0.0365(16) Uani 1 1 d . .
C21 C 0.1624(14) 0.5935(7) 0.1528(6) 0.058(2) Uani 1 1 d . .
H21A H 0.1482 0.6701 0.1501 0.088 Uiso 1 1 calc R U
H21B H 0.0119 0.5474 0.1511 0.088 Uiso 1 1 calc R U
H21C H 0.2218 0.5539 0.0941 0.088 Uiso 1 1 calc R U
C22 C 0.5573(13) 0.6840(6) 0.2556(6) 0.052(2) Uani 1 1 d . .
H22A H 0.5367 0.7601 0.2539 0.079 Uiso 1 1 calc R U
H22B H 0.6203 0.6475 0.1970 0.079 Uiso 1 1 calc R U
H22C H 0.6630 0.6935 0.3187 0.079 Uiso 1 1 calc R U
C23 C 0.2312(14) 0.6652(6) 0.3434(6) 0.051(2) Uani 1 1 d . .
H23A H 0.2213 0.7436 0.3443 0.077 Uiso 1 1 calc R U
H23B H 0.3328 0.6697 0.4060 0.077 Uiso 1 1 calc R U
H23C H 0.0785 0.6194 0.3389 0.077 Uiso 1 1 calc R U
C3 C 0.4145(12) 0.2272(6) 0.0600(5) 0.0370(17) Uani 1 1 d . .
C31 C 0.2762(15) 0.1036(6) 0.0338(5) 0.053(2) Uani 1 1 d . .
H31A H 0.2496 0.0644 -0.0397 0.080 Uiso 1 1 calc R U
H31B H 0.1291 0.1048 0.0546 0.080 Uiso 1 1 calc R U
H31C H 0.3608 0.0617 0.0698 0.080 Uiso 1 1 calc R U
C32 C 0.6491(13) 0.2268(7) 0.0309(6) 0.051(2) Uani 1 1 d . .
H32A H 0.6276 0.1857 -0.0421 0.077 Uiso 1 1 calc R U
H32B H 0.7340 0.1876 0.0696 0.077 Uiso 1 1 calc R U
H32C H 0.7353 0.3069 0.0466 0.077 Uiso 1 1 calc R U
C33 C 0.2862(14) 0.2939(7) 0.0045(5) 0.052(2) Uani 1 1 d . .
H33A H 0.2569 0.2543 -0.0691 0.077 Uiso 1 1 calc R U
H33B H 0.3788 0.3728 0.0208 0.077 Uiso 1 1 calc R U
H33C H 0.1405 0.2974 0.0262 0.077 Uiso 1 1 calc R U
C4 C 0.8189(11) 0.4374(5) 0.4168(4) 0.0298(15) Uani 1 1 d . .
C5 C 0.8116(12) 0.5444(6) 0.4815(5) 0.0356(17) Uani 1 1 d . .
H5A H 0.6824 0.5758 0.4699 0.043 Uiso 1 1 calc R U
C6 C 0.9922(12) 0.6064(6) 0.5633(5) 0.0362(17) Uani 1 1 d . .
H6A H 0.9854 0.6803 0.6063 0.043 Uiso 1 1 calc R U
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'
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
N2 P1 N3 105.7(3) .
N2 P1 N4 106.3(3) .
N3 P1 N4 79.5(2) .
N2 P1 P2 118.9(2) .
N1 P2 N4 104.8(3) .
N1 P2 N3 103.9(3) .
N4 P2 N3 79.9(2) .
N1 P2 P1 116.8(2) .
C1 N1 P2 130.9(5) .
C1 N1 H1 118(6) .
P2 N1 H1 111(5) .
C2 N2 P1 128.4(5) .
C2 N2 H2 112(5) .
P1 N2 H2 118(5) .
C3 N3 P2 123.3(4) .
C3 N3 P1 122.9(4) .
P2 N3 P1 98.9(3) .
C4 N4 P2 127.0(4) .
C4 N4 P1 122.8(4) .
P2 N4 P1 99.1(3) .
N1 C1 C13 110.3(6) .
N1 C1 C11 110.6(6) .
C13 C1 C11 110.3(7) .
N1 C1 C12 108.2(6) .
C13 C1 C12 109.1(7) .
C11 C1 C12 108.3(7) .
C1 C11 H11A 109.5 .
C1 C11 H11B 109.5 .
H11A C11 H11B 109.5 .
C1 C11 H11C 109.5 .
H11A C11 H11C 109.5 .
H11B C11 H11C 109.5 .
C1 C12 H12A 109.5 .
C1 C12 H12B 109.5 .
H12A C12 H12B 109.5 .
C1 C12 H12C 109.5 .
H12A C12 H12C 109.5 .
H12B C12 H12C 109.5 .
C1 C13 H13A 109.5 .
C1 C13 H13B 109.5 .
H13A C13 H13B 109.5 .
C1 C13 H13C 109.5 .
H13A C13 H13C 109.5 .
H13B C13 H13C 109.5 .
N2 C2 C21 110.2(6) .
N2 C2 C22 110.6(6) .
C21 C2 C22 109.2(6) .
N2 C2 C23 108.1(5) .
C21 C2 C23 110.0(6) .
C22 C2 C23 108.8(6) .
C2 C21 H21A 109.5 .
C2 C21 H21B 109.5 .
H21A C21 H21B 109.5 .
C2 C21 H21C 109.5 .
H21A C21 H21C 109.5 .
H21B C21 H21C 109.5 .
C2 C22 H22A 109.5 .
C2 C22 H22B 109.5 .
H22A C22 H22B 109.5 .
C2 C22 H22C 109.5 .
H22A C22 H22C 109.5 .
H22B C22 H22C 109.5 .
C2 C23 H23A 109.5 .
C2 C23 H23B 109.5 .
H23A C23 H23B 109.5 .
C2 C23 H23C 109.5 .
H23A C23 H23C 109.5 .
H23B C23 H23C 109.5 .
N3 C3 C31 107.8(5) .
N3 C3 C33 108.4(5) .
C31 C3 C33 110.4(6) .
N3 C3 C32 110.2(6) .
C31 C3 C32 110.2(6) .
C33 C3 C32 109.9(6) .
C3 C31 H31A 109.5 .
C3 C31 H31B 109.5 .
H31A C31 H31B 109.5 .
C3 C31 H31C 109.5 .
H31A C31 H31C 109.5 .
H31B C31 H31C 109.5 .
C3 C32 H32A 109.5 .
C3 C32 H32B 109.5 .
H32A C32 H32B 109.5 .
C3 C32 H32C 109.5 .
H32A C32 H32C 109.5 .
H32B C32 H32C 109.5 .
C3 C33 H33A 109.5 .
C3 C33 H33B 109.5 .
H33A C33 H33B 109.5 .
C3 C33 H33C 109.5 .
H33A C33 H33C 109.5 .
H33B C33 H33C 109.5 .
C6 C4 C5 118.3(6) 2_766
C6 C4 N4 122.4(6) 2_766
C5 C4 N4 119.3(6) .
C4 C5 C6 120.5(6) .
C4 C5 H5A 119.8 .
C6 C5 H5A 119.8 .
C4 C6 C5 121.3(6) 2_766
C4 C6 H6A 119.4 2_766
C5 C6 H6A 119.4 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
P1 N2 1.654(6) .
P1 N3 1.734(5) .
P1 N4 1.738(5) .
P1 P2 2.636(2) .
P2 N1 1.658(6) .
P2 N4 1.725(5) .
P2 N3 1.734(5) .
N1 C1 1.466(9) .
N1 H1 0.879(10) .
N2 C2 1.464(8) .
N2 H2 0.879(10) .
N3 C3 1.494(8) .
N4 C4 1.434(8) .
C1 C13 1.509(10) .
C1 C11 1.520(11) .
C1 C12 1.524(10) .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C2 C21 1.528(10) .
C2 C22 1.528(10) .
C2 C23 1.533(10) .
C21 H21A 0.9800 .
C21 H21B 0.9800 .
C21 H21C 0.9800 .
C22 H22A 0.9800 .
C22 H22B 0.9800 .
C22 H22C 0.9800 .
C23 H23A 0.9800 .
C23 H23B 0.9800 .
C23 H23C 0.9800 .
C3 C31 1.520(9) .
C3 C33 1.526(9) .
C3 C32 1.537(10) .
C31 H31A 0.9800 .
C31 H31B 0.9800 .
C31 H31C 0.9800 .
C32 H32A 0.9800 .
C32 H32B 0.9800 .
C32 H32C 0.9800 .
C33 H33A 0.9800 .
C33 H33B 0.9800 .
C33 H33C 0.9800 .
C4 C6 1.381(9) 2_766
C4 C5 1.385(9) .
C5 C6 1.392(9) .
C5 H5A 0.9500 .
C6 C4 1.381(9) 2_766
C6 H6A 0.9500 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
N4 P2 N1 C1 -135.5(7) . .
N3 P2 N1 C1 141.5(7) . .
P1 P2 N1 C1 -177.3(6) . .
N3 P1 N2 C2 -143.0(6) . .
N4 P1 N2 C2 133.6(6) . .
P2 P1 N2 C2 175.3(5) . .
N1 P2 N3 C3 -105.2(5) . .
N4 P2 N3 C3 151.9(5) . .
P1 P2 N3 C3 139.7(6) . .
N1 P2 N3 P1 115.2(3) . .
N4 P2 N3 P1 12.3(3) . .
N2 P1 N3 C3 103.7(5) . .
N4 P1 N3 C3 -152.1(5) . .
P2 P1 N3 C3 -139.9(6) . .
N2 P1 N3 P2 -116.4(3) . .
N4 P1 N3 P2 -12.2(3) . .
N1 P2 N4 C4 102.1(6) . .
N3 P2 N4 C4 -156.1(6) . .
P1 P2 N4 C4 -143.8(7) . .
N1 P2 N4 P1 -114.1(3) . .
N3 P2 N4 P1 -12.2(3) . .
N2 P1 N4 C4 -98.4(6) . .
N3 P1 N4 C4 158.1(5) . .
P2 P1 N4 C4 145.9(7) . .
N2 P1 N4 P2 115.7(3) . .
N3 P1 N4 P2 12.3(3) . .
P2 N1 C1 C13 16.1(11) . .
P2 N1 C1 C11 -106.3(9) . .
P2 N1 C1 C12 135.3(7) . .
P1 N2 C2 C21 101.9(7) . .
P1 N2 C2 C22 -18.9(9) . .
P1 N2 C2 C23 -137.9(6) . .
P2 N3 C3 C31 56.2(7) . .
P1 N3 C3 C31 -173.4(5) . .
P2 N3 C3 C33 175.7(5) . .
P1 N3 C3 C33 -53.9(7) . .
P2 N3 C3 C32 -64.0(7) . .
P1 N3 C3 C32 66.3(7) . .
P2 N4 C4 C6 20.9(9) . 2_766
P1 N4 C4 C6 -115.3(6) . 2_766
P2 N4 C4 C5 -160.5(5) . .
P1 N4 C4 C5 63.4(8) . .
C6 C4 C5 C6 0.9(11) 2_766 .
N4 C4 C5 C6 -177.8(6) . .
C4 C5 C6 C4 -0.9(11) . 2_766
