#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:07:43 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178550 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/57/4065795.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_4065795
loop_
_publ_author_name
'Boomishankar, Ramamoorthy'
'Richards, Philip I.'
'Gupta, Arvind K.'
'Steiner, Alexander'
_publ_section_title
;
 Magnesium and Titanium Complexes of Polyanionic Phosphazenate Ligands
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2515
_journal_paper_doi               10.1021/om100130k
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C56 H132 Mg2 N18 O2 P6'
_chemical_formula_weight         1324.24
_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                100.740(8)
_cell_angle_beta                 111.112(9)
_cell_angle_gamma                115.064(7)
_cell_formula_units_Z            1
_cell_length_a                   13.088(6)
_cell_length_b                   13.533(6)
_cell_length_c                   13.655(6)
_cell_measurement_temperature    123(2)
_cell_volume                     1872.2(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker Smart Apex'
_diffrn_measurement_method       ω
_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  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0364
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            9752
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.70
_exptl_absorpt_coefficient_mu    0.210
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.615
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.455
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         6504
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0384
_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)+(0.0556P)²+1.0374P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1026
_refine_ls_wR_factor_ref         0.1056
_reflns_number_gt                5879
_reflns_number_total             6504
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100130k_si_001.cif
_cod_data_source_block           bsr66a
_cod_original_cell_volume        1872.2(14)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4065795
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
Mg1 Mg -0.08496(5) 0.55923(5) -0.01679(4) 0.01654(14) Uani 1 1 d .
P1 P 0.03683(4) 0.56703(4) 0.20794(3) 0.01653(12) Uani 1 1 d .
P2 P 0.18706(4) 0.72017(4) 0.13177(3) 0.01633(12) Uani 1 1 d .
P3 P 0.23106(4) 0.80517(4) 0.35570(3) 0.01754(12) Uani 1 1 d .
N1 N 0.10898(13) 0.58580(12) 0.12970(11) 0.0163(3) Uani 1 1 d .
N2 N 0.26635(13) 0.82289(12) 0.25725(12) 0.0199(3) Uani 1 1 d .
N3 N 0.12250(14) 0.67549(13) 0.33075(12) 0.0201(3) Uani 1 1 d .
N4 N -0.10533(13) 0.53586(13) 0.12079(12) 0.0200(3) Uani 1 1 d .
N5 N 0.01670(15) 0.44896(14) 0.23580(13) 0.0233(3) Uani 1 1 d .
H5 H -0.034(2) 0.389(2) 0.185(2) 0.028(6) Uiso 1 1 d .
N6 N 0.07464(13) 0.71905(12) 0.02941(12) 0.0185(3) Uani 1 1 d .
N7 N 0.29468(14) 0.73027(14) 0.09187(13) 0.0231(3) Uani 1 1 d .
H7 H 0.263(2) 0.684(2) 0.026(2) 0.031(6) Uiso 1 1 d .
N8 N 0.18209(16) 0.89087(14) 0.39965(13) 0.0242(3) Uani 1 1 d .
H8 H 0.103(2) 0.8602(19) 0.3681(18) 0.029(6) Uiso 1 1 d .
N9 N 0.37401(15) 0.86159(14) 0.46817(12) 0.0231(3) Uani 1 1 d .
H9 H 0.434(3) 0.877(2) 0.457(2) 0.044(7) Uiso 1 1 d .
C41 C -0.20056(17) 0.50996(17) 0.15990(15) 0.0249(4) Uani 1 1 d .
H41A H -0.1551 0.5384 0.2444 0.030 Uiso 1 1 calc R
H41B H -0.2614 0.4227 0.1275 0.030 Uiso 1 1 calc R
C42 C -0.27711(18) 0.56787(18) 0.12540(16) 0.0289(4) Uani 1 1 d .
H42 H -0.3157 0.5442 0.0407 0.035 Uiso 1 1 calc R
C43 C -0.3879(2) 0.5232(2) 0.15255(19) 0.0423(5) Uani 1 1 d .
H43A H -0.4426 0.4361 0.1145 0.063 Uiso 1 1 calc R
H43B H -0.4400 0.5571 0.1250 0.063 Uiso 1 1 calc R
H43C H -0.3521 0.5478 0.2356 0.063 Uiso 1 1 calc R
C44 C -0.1902(2) 0.7025(2) 0.1833(2) 0.0420(5) Uani 1 1 d .
H44A H -0.2421 0.7374 0.1596 0.063 Uiso 1 1 calc R
H44B H -0.1231 0.7296 0.1610 0.063 Uiso 1 1 calc R
H44C H -0.1492 0.7277 0.2666 0.063 Uiso 1 1 calc R
C51 C 0.10008(18) 0.44452(16) 0.33684(15) 0.0259(4) Uani 1 1 d .
H51A H 0.1786 0.5252 0.3867 0.031 Uiso 1 1 calc R
H51B H 0.1281 0.3914 0.3131 0.031 Uiso 1 1 calc R
C52 C 0.0358(2) 0.4008(2) 0.40507(17) 0.0403(5) Uani 1 1 d .
H52 H 0.0044 0.4528 0.4260 0.048 Uiso 1 1 calc R
C53 C 0.1316(3) 0.4085(2) 0.5145(2) 0.0710(10) Uani 1 1 d .
H53A H 0.0882 0.3798 0.5576 0.107 Uiso 1 1 calc R
H53B H 0.2039 0.4915 0.5611 0.107 Uiso 1 1 calc R
H53C H 0.1647 0.3593 0.4954 0.107 Uiso 1 1 calc R
C54 C -0.0800(2) 0.2730(3) 0.3355(2) 0.0627(8) Uani 1 1 d .
H54A H -0.1196 0.2469 0.3819 0.094 Uiso 1 1 calc R
H54B H -0.0509 0.2211 0.3132 0.094 Uiso 1 1 calc R
H54C H -0.1439 0.2688 0.2666 0.094 Uiso 1 1 calc R
C61 C 0.10915(17) 0.81052(15) -0.01622(14) 0.0214(4) Uani 1 1 d .
H61A H 0.0284 0.7925 -0.0805 0.026 Uiso 1 1 calc R
H61B H 0.1637 0.8036 -0.0485 0.026 Uiso 1 1 calc R
C62 C 0.18069(17) 0.93983(15) 0.06686(15) 0.0234(4) Uani 1 1 d .
H62 H 0.2648 0.9599 0.1296 0.028 Uiso 1 1 calc R
C63 C 0.1036(2) 0.95883(17) 0.12017(17) 0.0310(4) Uani 1 1 d .
H63A H 0.0862 0.9061 0.1603 0.047 Uiso 1 1 calc R
H63B H 0.0213 0.9409 0.0600 0.047 Uiso 1 1 calc R
H63C H 0.1534 1.0419 0.1747 0.047 Uiso 1 1 calc R
C64 C 0.2104(2) 1.02021(17) 0.00345(18) 0.0303(4) Uani 1 1 d .
H64A H 0.2603 1.0059 -0.0299 0.045 Uiso 1 1 calc R
H64B H 0.2610 1.1037 0.0572 0.045 Uiso 1 1 calc R
H64C H 0.1290 1.0027 -0.0577 0.045 Uiso 1 1 calc R
C71 C 0.43349(16) 0.78652(16) 0.16213(15) 0.0233(4) Uani 1 1 d .
H71A H 0.4563 0.7262 0.1484 0.028 Uiso 1 1 calc R
H71B H 0.4573 0.8159 0.2439 0.028 Uiso 1 1 calc R
C72 C 0.51223(17) 0.88974(17) 0.13842(16) 0.0263(4) Uani 1 1 d .
H72 H 0.4934 0.9527 0.1584 0.032 Uiso 1 1 calc R
C73 C 0.65660(18) 0.94287(19) 0.21410(18) 0.0368(5) Uani 1 1 d .
H73A H 0.6784 0.9669 0.2947 0.055 Uiso 1 1 calc R
H73B H 0.7065 1.0126 0.2019 0.055 Uiso 1 1 calc R
H73C H 0.6777 0.8833 0.1944 0.055 Uiso 1 1 calc R
C74 C 0.4754(2) 0.8519(2) 0.01245(17) 0.0381(5) Uani 1 1 d .
H74A H 0.5279 0.9204 0.0002 0.057 Uiso 1 1 calc R
H74B H 0.3834 0.8219 -0.0345 0.057 Uiso 1 1 calc R
H74C H 0.4914 0.7889 -0.0094 0.057 Uiso 1 1 calc R
C81 C 0.25665(18) 1.01959(16) 0.43966(16) 0.0277(4) Uani 1 1 d .
H81A H 0.2625 1.0409 0.3755 0.033 Uiso 1 1 calc R
H81B H 0.3458 1.0515 0.5006 0.033 Uiso 1 1 calc R
C82 C 0.1968(2) 1.07750(18) 0.48645(17) 0.0315(4) Uani 1 1 d .
H82 H 0.1797 1.0456 0.5430 0.038 Uiso 1 1 calc R
C83 C 0.0689(2) 1.0493(2) 0.3933(2) 0.0431(5) Uani 1 1 d .
H83A H 0.0084 0.9628 0.3538 0.065 Uiso 1 1 calc R
H83B H 0.0837 1.0822 0.3382 0.065 Uiso 1 1 calc R
H83C H 0.0321 1.0848 0.4279 0.065 Uiso 1 1 calc R
C84 C 0.2929(2) 1.2111(2) 0.5495(2) 0.0483(6) Uani 1 1 d .
H84A H 0.3746 1.2274 0.6089 0.073 Uiso 1 1 calc R
H84B H 0.2573 1.2474 0.5849 0.073 Uiso 1 1 calc R
H84C H 0.3089 1.2449 0.4951 0.073 Uiso 1 1 calc R
C91 C 0.39897(18) 0.86960(16) 0.58303(14) 0.0247(4) Uani 1 1 d .
H91A H 0.3415 0.8903 0.6002 0.030 Uiso 1 1 calc R
H91B H 0.4896 0.9354 0.6385 0.030 Uiso 1 1 calc R
C92 C 0.37858(19) 0.75676(17) 0.60139(15) 0.0289(4) Uani 1 1 d .
H92 H 0.2844 0.6932 0.5523 0.035 Uiso 1 1 calc R
C93 C 0.4155(2) 0.7788(2) 0.72638(17) 0.0371(5) Uani 1 1 d .
H93A H 0.4021 0.7059 0.7379 0.056 Uiso 1 1 calc R
H93B H 0.3611 0.8017 0.7455 0.056 Uiso 1 1 calc R
H93C H 0.5068 0.8429 0.7761 0.056 Uiso 1 1 calc R
C94 C 0.4554(2) 0.7136(2) 0.56728(18) 0.0386(5) Uani 1 1 d .
H94A H 0.4400 0.6409 0.5801 0.058 Uiso 1 1 calc R
H94B H 0.5481 0.7753 0.6137 0.058 Uiso 1 1 calc R
H94C H 0.4278 0.6967 0.4860 0.058 Uiso 1 1 calc R
O1 O -0.23663(12) 0.56598(11) -0.12537(10) 0.0245(3) Uani 1 1 d .
C11 C -0.24786(18) 0.66836(17) -0.10734(16) 0.0279(4) Uani 1 1 d .
H11A H -0.1628 0.7419 -0.0511 0.034 Uiso 1 1 calc R
H11B H -0.3102 0.6590 -0.0795 0.034 Uiso 1 1 calc R
C12 C -0.2962(2) 0.67204(18) -0.22368(17) 0.0354(5) Uani 1 1 d .
H12A H -0.2240 0.7111 -0.2392 0.043 Uiso 1 1 calc R
H12B H -0.3424 0.7147 -0.2308 0.043 Uiso 1 1 calc R
C13 C -0.38866(19) 0.54033(18) -0.30441(16) 0.0311(4) Uani 1 1 d .
H13A H -0.4791 0.5138 -0.3237 0.037 Uiso 1 1 calc R
H13B H -0.3843 0.5255 -0.3762 0.037 Uiso 1 1 calc R
C14 C -0.34127(18) 0.47619(16) -0.23742(16) 0.0285(4) Uani 1 1 d .
H14A H -0.4123 0.4158 -0.2311 0.034 Uiso 1 1 calc R
H14B H -0.3103 0.4358 -0.2763 0.034 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'
Mg Mg 0.0486 0.0363 '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
N6 Mg1 N4 112.56(6) . .
N6 Mg1 O1 103.70(7) . .
N4 Mg1 O1 110.23(6) . .
N6 Mg1 N1 114.61(7) . 2_565
N4 Mg1 N1 114.86(7) . 2_565
O1 Mg1 N1 99.34(6) . 2_565
N6 Mg1 N1 69.03(6) . .
N4 Mg1 N1 68.60(6) . .
O1 Mg1 N1 170.45(5) . .
N1 Mg1 N1 89.52(6) 2_565 .
N6 Mg1 P2 33.72(4) . .
N4 Mg1 P2 89.62(5) . .
O1 Mg1 P2 136.68(5) . .
N1 Mg1 P2 106.63(5) 2_565 .
N1 Mg1 P2 35.43(4) . .
N6 Mg1 P1 89.81(5) . .
N4 Mg1 P1 33.55(5) . .
O1 Mg1 P1 142.30(4) . .
N1 Mg1 P1 106.74(5) 2_565 .
N1 Mg1 P1 35.17(3) . .
P2 Mg1 P1 59.67(2) . .
N6 Mg1 Mg1 89.98(6) . 2_565
N4 Mg1 Mg1 89.82(5) . 2_565
O1 Mg1 Mg1 148.26(5) . 2_565
N1 Mg1 Mg1 49.08(4) 2_565 2_565
N1 Mg1 Mg1 40.44(4) . 2_565
P2 Mg1 Mg1 64.53(4) . 2_565
P1 Mg1 Mg1 64.48(2) . 2_565
N3 P1 N4 119.75(8) . .
N3 P1 N5 104.95(8) . .
N4 P1 N5 107.00(8) . .
N3 P1 N1 112.13(8) . .
N4 P1 N1 102.19(8) . .
N5 P1 N1 110.71(8) . .
N3 P1 Mg1 130.53(6) . .
N4 P1 Mg1 44.60(5) . .
N5 P1 Mg1 124.23(6) . .
N1 P1 Mg1 57.81(6) . .
N2 P2 N6 119.52(8) . .
N2 P2 N7 106.30(8) . .
N6 P2 N7 106.68(8) . .
N2 P2 N1 112.38(8) . .
N6 P2 N1 102.37(7) . .
N7 P2 N1 109.23(8) . .
N2 P2 Mg1 130.68(6) . .
N6 P2 Mg1 44.45(6) . .
N7 P2 Mg1 122.76(7) . .
N1 P2 Mg1 58.12(5) . .
N3 P3 N2 117.85(8) . .
N3 P3 N9 114.88(8) . .
N2 P3 N9 102.79(9) . .
N3 P3 N8 103.32(9) . .
N2 P3 N8 115.25(8) . .
N9 P3 N8 102.02(9) . .
P1 N1 P2 118.52(8) . .
P1 N1 Mg1 120.78(8) . 2_565
P2 N1 Mg1 120.34(8) . 2_565
P1 N1 Mg1 87.02(7) . .
P2 N1 Mg1 86.45(6) . .
Mg1 N1 Mg1 90.48(6) 2_565 .
P3 N2 P2 122.69(9) . .
P3 N3 P1 123.01(9) . .
C41 N4 P1 118.30(12) . .
C41 N4 Mg1 139.66(12) . .
P1 N4 Mg1 101.85(8) . .
C51 N5 P1 127.80(13) . .
C61 N6 P2 119.93(12) . .
C61 N6 Mg1 137.27(11) . .
P2 N6 Mg1 101.84(8) . .
C71 N7 P2 129.00(13) . .
C81 N8 P3 123.13(13) . .
C91 N9 P3 126.23(14) . .
N4 C41 C42 112.79(15) . .
C44 C42 C41 111.27(16) . .
C44 C42 C43 110.83(17) . .
C41 C42 C43 110.44(17) . .
N5 C51 C52 113.43(17) . .
C51 C52 C53 110.6(2) . .
C51 C52 C54 111.25(18) . .
C53 C52 C54 109.5(2) . .
N6 C61 C62 117.26(15) . .
C63 C62 C64 111.42(15) . .
C63 C62 C61 111.62(15) . .
C64 C62 C61 108.85(15) . .
N7 C71 C72 113.26(15) . .
C71 C72 C74 111.63(16) . .
C71 C72 C73 110.12(16) . .
C74 C72 C73 110.69(16) . .
N8 C81 C82 112.46(16) . .
C84 C82 C83 110.78(18) . .
C84 C82 C81 109.56(18) . .
C83 C82 C81 112.49(17) . .
N9 C91 C92 114.76(15) . .
C94 C92 C91 111.64(17) . .
C94 C92 C93 110.64(17) . .
C91 C92 C93 109.69(16) . .
C11 O1 C14 107.94(13) . .
C11 O1 Mg1 125.03(10) . .
C14 O1 Mg1 126.67(11) . .
O1 C11 C12 104.06(15) . .
C11 C12 C13 102.95(16) . .
C14 C13 C12 104.50(15) . .
O1 C14 C13 106.55(15) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mg1 N6 2.0381(17) .
Mg1 N4 2.0521(17) .
Mg1 O1 2.0570(15) .
Mg1 N1 2.0804(16) 2_565
Mg1 N1 2.4238(17) .
Mg1 P2 2.8487(13) .
Mg1 P1 2.8603(13) .
Mg1 Mg1 3.2073(15) 2_565
P1 N3 1.5992(15) .
P1 N4 1.6151(16) .
P1 N5 1.6460(17) .
P1 N1 1.6499(15) .
P2 N2 1.5982(15) .
P2 N6 1.6158(15) .
P2 N7 1.6483(16) .
P2 N1 1.6545(15) .
P3 N3 1.5908(16) .
P3 N2 1.5975(16) .
P3 N9 1.6506(16) .
P3 N8 1.6624(16) .
N1 Mg1 2.0804(16) 2_565
N4 C41 1.463(2) .
N5 C51 1.449(2) .
N6 C61 1.463(2) .
N7 C71 1.450(2) .
N8 C81 1.451(2) .
N9 C91 1.455(2) .
C41 C42 1.518(3) .
C42 C44 1.516(3) .
C42 C43 1.527(3) .
C51 C52 1.508(3) .
C52 C53 1.516(3) .
C52 C54 1.523(4) .
C61 C62 1.527(2) .
C62 C63 1.515(3) .
C62 C64 1.523(3) .
C71 C72 1.519(3) .
C72 C74 1.523(3) .
C72 C73 1.523(3) .
C81 C82 1.526(3) .
C82 C84 1.519(3) .
C82 C83 1.520(3) .
C91 C92 1.520(3) .
C92 C94 1.518(3) .
C92 C93 1.526(3) .
O1 C11 1.440(2) .
O1 C14 1.442(2) .
C11 C12 1.503(3) .
C12 C13 1.528(3) .
C13 C14 1.523(3) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N7 H7 N4 0.82(2) 2.59(2) 3.302(2) 145(2) 2_565
N5 H5 N6 0.76(2) 2.75(2) 3.350(3) 136(2) 2_565
