#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:16:38 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179807 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/03/7010304.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_7010304
loop_
_publ_author_name
'Moser, Daniel F.'
'Carrow, Christopher J.'
'Stahl, Lothar'
'Staples, Richard J.'
_publ_section_title
;
 Titanium complexes of bis(1°-amido)cyclodiphosph(III)azanes and
 bis(1°-amido)cyclodiphosph(V)azanes: facial versus lateral
 coordination †
;
_journal_issue                   8
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1246
_journal_paper_doi               10.1039/b007877h
_journal_year                    2001
_chemical_formula_sum            'C30 H52 N6 P2'
_chemical_formula_weight         558.72
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 90.838(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.144(3)
_cell_length_b                   20.5351(18)
_cell_length_c                   13.4541(12)
_cell_measurement_reflns_used    46
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.49
_cell_measurement_theta_min      3.73
_cell_volume                     3354.8(9)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '2θ/ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0180
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7190
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.81
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.157
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.273
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         5887
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0501
_refine_ls_shift/su_max          0.092
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0829P)²+0.9037P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1328
_refine_ls_wR_factor_ref         0.1526
_reflns_number_gt                4244
_reflns_number_total             5887
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b007877h.txt
_cod_data_source_block           4
_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      P2(1)/n
_cod_database_code               7010304
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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 0.14497(5) 0.19944(3) 0.60602(4) 0.03952(19) Uani 1 1 d . . .
P2 P 0.21677(5) 0.09529(3) 0.68455(5) 0.0438(2) Uani 1 1 d . . .
N3 N 0.2379(2) 0.24583(11) 0.55603(17) 0.0482(5) Uani 1 1 d . . .
N1 N 0.18783(18) 0.17242(10) 0.71868(13) 0.0471(5) Uani 1 1 d . A .
N2 N 0.17046(17) 0.12147(9) 0.57253(14) 0.0438(5) Uani 1 1 d . . .
N6 N 0.16965(18) 0.03621(10) 0.74046(17) 0.0542(6) Uani 1 1 d . . .
C1 C 0.2013(2) 0.20659(13) 0.81588(17) 0.0518(6) Uani 1 1 d . . .
N4 N 0.3493(2) 0.08226(13) 0.67742(19) 0.0562(6) Uani 1 1 d . . .
C63 C -0.1319(2) 0.04170(13) 0.78613(19) 0.0518(6) Uani 1 1 d . . .
H63 H -0.1935 0.0655 0.7663 0.062 Uiso 1 1 calc R . .
C61 C 0.0639(2) 0.02360(12) 0.77404(17) 0.0454(6) Uani 1 1 d . . .
C2 C 0.1756(2) 0.09002(13) 0.47268(19) 0.0556(7) Uani 1 1 d . . .
N5 N 0.03582(18) 0.23410(11) 0.59159(17) 0.0560(6) Uani 1 1 d . . .
C51 C -0.0758(2) 0.23056(13) 0.61042(18) 0.0486(6) Uani 1 1 d . . .
C62 C -0.0310(2) 0.05791(12) 0.74785(18) 0.0508(6) Uani 1 1 d . . .
H62 H -0.0261 0.0925 0.7035 0.061 Uiso 1 1 calc R . .
C3 C 0.2310(2) 0.31066(12) 0.5070(2) 0.0537(7) Uani 1 1 d . . .
C56 C -0.1430(2) 0.17858(14) 0.5813(2) 0.0577(7) Uani 1 1 d . . .
H56 H -0.1114 0.1420 0.5526 0.069 Uiso 1 1 calc R . .
C64 C -0.1448(2) -0.00863(13) 0.85294(19) 0.0520(6) Uani 1 1 d . . .
C66 C 0.0508(2) -0.02759(14) 0.8406(2) 0.0644(8) Uani 1 1 d . . .
H66 H 0.1118 -0.0522 0.8598 0.077 Uiso 1 1 calc R . .
C52 C -0.1287(2) 0.28338(15) 0.6552(2) 0.0632(7) Uani 1 1 d . . .
H52 H -0.0869 0.3187 0.6768 0.076 Uiso 1 1 calc R . .
C41 C 0.5386(3) 0.04761(18) 0.6851(3) 0.0829(10) Uani 1 1 d . . .
H41A H 0.5396 0.0508 0.6139 0.124 Uiso 1 1 calc R . .
H41B H 0.5890 0.0143 0.7067 0.124 Uiso 1 1 calc R . .
H41C H 0.5602 0.0886 0.7137 0.124 Uiso 1 1 calc R . .
C54 C -0.3070(2) 0.23338(18) 0.6374(2) 0.0683(9) Uani 1 1 d . . .
C4 C 0.4232(2) 0.03045(14) 0.7182(2) 0.0615(7) Uani 1 1 d . . .
C65 C -0.0507(2) -0.04245(15) 0.8784(2) 0.0683(8) Uani 1 1 d . . .
H65 H -0.0560 -0.0768 0.9231 0.082 Uiso 1 1 calc R . .
C55 C -0.2557(2) 0.18044(17) 0.5943(2) 0.0670(8) Uani 1 1 d . . .
H55 H -0.2981 0.1452 0.5736 0.080 Uiso 1 1 calc R . .
C21 C 0.2846(3) 0.10501(18) 0.4230(2) 0.0824(10) Uani 1 1 d . . .
H21A H 0.2910 0.1511 0.4129 0.124 Uiso 1 1 calc R . .
H21B H 0.2873 0.0831 0.3600 0.124 Uiso 1 1 calc R . .
H21C H 0.3444 0.0903 0.4647 0.124 Uiso 1 1 calc R . .
C53 C -0.2405(3) 0.28422(17) 0.6678(2) 0.0696(8) Uani 1 1 d . . .
H53 H -0.2724 0.3202 0.6978 0.083 Uiso 1 1 calc R . .
C43 C 0.4190(3) 0.02900(19) 0.8314(2) 0.0839(10) Uani 1 1 d . . .
H43A H 0.4401 0.0708 0.8573 0.126 Uiso 1 1 calc R . .
H43B H 0.4687 -0.0036 0.8564 0.126 Uiso 1 1 calc R . .
H43C H 0.3455 0.0189 0.8516 0.126 Uiso 1 1 calc R . .
C31 C 0.3484(3) 0.32882(17) 0.4811(3) 0.0839(10) Uani 1 1 d . . .
H31A H 0.3936 0.3280 0.5403 0.126 Uiso 1 1 calc R . .
H31B H 0.3494 0.3717 0.4529 0.126 Uiso 1 1 calc R . .
H31C H 0.3765 0.2982 0.4340 0.126 Uiso 1 1 calc R . .
C22 C 0.1647(4) 0.01627(15) 0.4880(3) 0.0882(11) Uani 1 1 d . . .
H22A H 0.2257 0.0008 0.5275 0.132 Uiso 1 1 calc R . .
H22B H 0.1643 -0.0052 0.4246 0.132 Uiso 1 1 calc R . .
H22C H 0.0971 0.0071 0.5214 0.132 Uiso 1 1 calc R . .
C67 C -0.2549(3) -0.02546(17) 0.8964(3) 0.0784(9) Uani 1 1 d . . .
H67A H -0.2857 -0.0622 0.8617 0.118 Uiso 1 1 calc R . .
H67B H -0.3036 0.0111 0.8897 0.118 Uiso 1 1 calc R . .
H67C H -0.2454 -0.0361 0.9655 0.118 Uiso 1 1 calc R . .
C33 C 0.1597(3) 0.30706(17) 0.4136(2) 0.0836(10) Uani 1 1 d . . .
H33A H 0.1899 0.2756 0.3688 0.125 Uiso 1 1 calc R . .
H33B H 0.1578 0.3490 0.3820 0.125 Uiso 1 1 calc R . .
H33C H 0.0863 0.2944 0.4308 0.125 Uiso 1 1 calc R . .
C32 C 0.1857(3) 0.36199(14) 0.5770(3) 0.0824(10) Uani 1 1 d . . .
H32A H 0.1113 0.3512 0.5935 0.124 Uiso 1 1 calc R . .
H32B H 0.1871 0.4038 0.5451 0.124 Uiso 1 1 calc R . .
H32C H 0.2302 0.3634 0.6366 0.124 Uiso 1 1 calc R . .
C42 C 0.3904(3) -0.03624(15) 0.6761(3) 0.0878(11) Uani 1 1 d . . .
H42A H 0.3163 -0.0462 0.6949 0.132 Uiso 1 1 calc R . .
H42B H 0.4394 -0.0689 0.7021 0.132 Uiso 1 1 calc R . .
H42C H 0.3948 -0.0353 0.6049 0.132 Uiso 1 1 calc R . .
C23 C 0.0812(3) 0.11478(17) 0.4077(2) 0.0761(9) Uani 1 1 d . . .
H23A H 0.0124 0.1025 0.4366 0.114 Uiso 1 1 calc R . .
H23B H 0.0863 0.0961 0.3426 0.114 Uiso 1 1 calc R . .
H23C H 0.0852 0.1614 0.4030 0.114 Uiso 1 1 calc R . .
C57 C -0.4302(3) 0.2363(2) 0.6489(3) 0.1037(14) Uani 1 1 d . . .
H57A H -0.4652 0.2124 0.5959 0.156 Uiso 1 1 calc R . .
H57B H -0.4540 0.2808 0.6466 0.156 Uiso 1 1 calc R . .
H57C H -0.4498 0.2175 0.7116 0.156 Uiso 1 1 calc R . .
C13 C 0.1135(4) 0.2597(2) 0.8229(3) 0.0748(16) Uani 0.823(8) 1 d P A 1
H13A H 0.1251 0.2916 0.7720 0.112 Uiso 0.823(8) 1 calc PR A 1
H13B H 0.1185 0.2802 0.8870 0.112 Uiso 0.823(8) 1 calc PR A 1
H13C H 0.0418 0.2407 0.8142 0.112 Uiso 0.823(8) 1 calc PR A 1
C12 C 0.1808(6) 0.1577(2) 0.8991(2) 0.0793(17) Uani 0.823(8) 1 d P A 1
H12A H 0.1059 0.1429 0.8953 0.119 Uiso 0.823(8) 1 calc PR A 1
H12B H 0.1941 0.1783 0.9623 0.119 Uiso 0.823(8) 1 calc PR A 1
H12C H 0.2296 0.1213 0.8921 0.119 Uiso 0.823(8) 1 calc PR A 1
C11 C 0.3144(4) 0.2342(4) 0.8211(4) 0.0880(19) Uani 0.823(8) 1 d P A 1
H11A H 0.3672 0.1999 0.8131 0.132 Uiso 0.823(8) 1 calc PR A 1
H11B H 0.3259 0.2549 0.8844 0.132 Uiso 0.823(8) 1 calc PR A 1
H11C H 0.3230 0.2658 0.7691 0.132 Uiso 0.823(8) 1 calc PR A 1
C11A C 0.299(3) 0.176(2) 0.8816(18) 0.12(2) Uani 0.17(2) 1 d P A 2
H11D H 0.2783 0.1340 0.9051 0.181 Uiso 0.42(13) 1 calc PR A 2
H11E H 0.3147 0.2043 0.9373 0.181 Uiso 0.34(9) 1 calc PR A 2
H11F H 0.3641 0.1724 0.8419 0.181 Uiso 0.41(10) 1 calc PR A 2
C12A C 0.090(3) 0.1995(18) 0.8612(19) 0.13(2) Uani 0.19(2) 1 d P A 2
H12D H 0.0345 0.2134 0.8143 0.189 Uiso 0.00(12) 1 calc PR A 2
H12E H 0.0864 0.2259 0.9199 0.189 Uiso 0.17(9) 1 calc PR A 2
H12F H 0.0779 0.1548 0.8784 0.189 Uiso 0.21(11) 1 calc PR A 2
C13A C 0.235(3) 0.2797(12) 0.8023(17) 0.120(19) Uani 0.21(2) 1 d P A 2
H13D H 0.2988 0.2821 0.7606 0.180 Uiso 0.15(11) 1 calc PR A 2
H13E H 0.2529 0.2983 0.8660 0.180 Uiso 0.17(9) 1 calc PR A 2
H13F H 0.1756 0.3033 0.7720 0.180 Uiso 0.14(12) 1 calc PR A 2
H3 H 0.294(2) 0.2342(13) 0.5612(19) 0.038(8) Uiso 1 1 d . . .
H4 H 0.375(3) 0.1063(16) 0.654(2) 0.065(11) Uiso 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
P P 0.1023 0.0942 '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'
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'
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
N5 P1 N3 106.41(13) . . ?
N5 P1 N1 121.80(12) . . ?
N3 P1 N1 110.86(12) . . ?
N5 P1 N2 124.98(12) . . ?
N3 P1 N2 108.22(11) . . ?
N1 P1 N2 82.71(10) . . ?
N5 P1 P2 138.17(9) . . ?
N3 P1 P2 115.42(10) . . ?
N1 P1 P2 41.34(7) . . ?
N2 P1 P2 41.39(7) . . ?
N6 P2 N4 105.81(13) . . ?
N6 P2 N1 121.70(11) . . ?
N4 P2 N1 112.23(12) . . ?
N6 P2 N2 124.39(12) . . ?
N4 P2 N2 108.35(12) . . ?
N1 P2 N2 82.88(9) . . ?
N6 P2 P1 137.68(9) . . ?
N4 P2 P1 116.51(10) . . ?
N1 P2 P1 41.38(7) . . ?
N2 P2 P1 41.52(7) . . ?
C3 N3 P1 132.2(2) . . ?
C1 N1 P2 131.28(17) . . ?
C1 N1 P1 131.37(17) . . ?
P2 N1 P1 97.28(10) . . ?
C2 N2 P2 130.35(17) . . ?
C2 N2 P1 131.22(17) . . ?
P2 N2 P1 97.09(10) . . ?
C61 N6 P2 130.96(18) . . ?
C11 C1 N1 108.1(2) . . ?
C11 C1 C12A 148.9(9) . . ?
N1 C1 C12A 102.9(10) . . ?
C11 C1 C12 112.1(4) . . ?
N1 C1 C12 108.5(2) . . ?
C12A C1 C12 58.7(16) . . ?
C11 C1 C13 111.7(4) . . ?
N1 C1 C13 108.8(2) . . ?
C12A C1 C13 53.8(15) . . ?
C12 C1 C13 107.6(3) . . ?
C11 C1 C13A 52.7(14) . . ?
N1 C1 C13A 112.0(8) . . ?
C12A C1 C13A 112.4(19) . . ?
C12 C1 C13A 139.5(9) . . ?
C13 C1 C13A 60.7(15) . . ?
C11 C1 C11A 56.1(17) . . ?
N1 C1 C11A 111.9(8) . . ?
C12A C1 C11A 114(2) . . ?
C12 C1 C11A 57.8(17) . . ?
C13 C1 C11A 139.2(8) . . ?
C13A C1 C11A 104(2) . . ?
C4 N4 P2 133.0(2) . . ?
C62 C63 C64 122.3(2) . . ?
C66 C61 N6 117.7(2) . . ?
C66 C61 C62 116.3(2) . . ?
N6 C61 C62 126.0(2) . . ?
N2 C2 C23 109.4(2) . . ?
N2 C2 C21 110.8(2) . . ?
C23 C2 C21 109.5(3) . . ?
N2 C2 C22 107.5(2) . . ?
C23 C2 C22 110.0(3) . . ?
C21 C2 C22 109.6(3) . . ?
C51 N5 P1 144.0(2) . . ?
N5 C51 C56 124.0(2) . . ?
N5 C51 C52 119.6(3) . . ?
C56 C51 C52 116.3(3) . . ?
C63 C62 C61 121.4(2) . . ?
N3 C3 C33 110.6(2) . . ?
N3 C3 C31 105.9(2) . . ?
C33 C3 C31 110.4(3) . . ?
N3 C3 C32 111.3(2) . . ?
C33 C3 C32 109.8(3) . . ?
C31 C3 C32 108.7(3) . . ?
C55 C56 C51 121.2(3) . . ?
C65 C64 C63 116.0(2) . . ?
C65 C64 C67 121.7(3) . . ?
C63 C64 C67 122.3(3) . . ?
C65 C66 C61 121.2(3) . . ?
C53 C52 C51 121.6(3) . . ?
C53 C54 C55 116.9(3) . . ?
C53 C54 C57 121.2(3) . . ?
C55 C54 C57 121.9(4) . . ?
N4 C4 C41 106.2(2) . . ?
N4 C4 C43 110.6(3) . . ?
C41 C4 C43 110.0(3) . . ?
N4 C4 C42 110.5(3) . . ?
C41 C4 C42 109.6(3) . . ?
C43 C4 C42 109.8(3) . . ?
C66 C65 C64 122.8(3) . . ?
C56 C55 C54 121.8(3) . . ?
C52 C53 C54 122.1(3) . . ?
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 N5 1.515(2) . ?
P1 N3 1.630(2) . ?
P1 N1 1.6892(19) . ?
P1 N2 1.693(2) . ?
P1 P2 2.5345(9) . ?
P2 N6 1.542(2) . ?
P2 N4 1.636(3) . ?
P2 N1 1.688(2) . ?
P2 N2 1.689(2) . ?
N3 C3 1.488(3) . ?
N1 C1 1.491(3) . ?
N2 C2 1.493(3) . ?
N6 C61 1.391(3) . ?
C1 C11 1.487(5) . ?
C1 C12A 1.50(3) . ?
C1 C12 1.527(5) . ?
C1 C13 1.530(5) . ?
C1 C13A 1.57(2) . ?
C1 C11A 1.60(2) . ?
N4 C4 1.491(4) . ?
C63 C62 1.377(4) . ?
C63 C64 1.380(4) . ?
C61 C66 1.392(3) . ?
C61 C62 1.392(4) . ?
C2 C23 1.519(4) . ?
C2 C21 1.524(4) . ?
C2 C22 1.534(4) . ?
N5 C51 1.385(3) . ?
C51 C56 1.396(4) . ?
C51 C52 1.401(4) . ?
C3 C33 1.517(4) . ?
C3 C31 1.519(4) . ?
C3 C32 1.522(4) . ?
C56 C55 1.382(4) . ?
C64 C65 1.377(4) . ?
C64 C67 1.507(4) . ?
C66 C65 1.375(4) . ?
C52 C53 1.371(4) . ?
C41 C4 1.518(4) . ?
C54 C53 1.379(5) . ?
C54 C55 1.385(5) . ?
C54 C57 1.507(4) . ?
C4 C43 1.525(4) . ?
C4 C42 1.532(4) . ?
