#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:01:37 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179227 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/47/4314719.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_4314719
loop_
_publ_author_name
'Jamie S. Ritch'
'Tristram Chivers'
'Kibriya Ahmad'
'Mohammad Afzaal'
'Paul O'Brien'
_publ_contact_author_address
;
Department of Chemistry
University of Calgary
2500 University Drive NW
Calgary AB  T2N 1N4
Canada
;
_publ_contact_author_name        'Prof. Tristram Chivers'
_publ_section_title
;
 Synthesis, Structures, and Multinuclear NMR Spectra of Tin(II) and
 Lead(II) Complexes of Tellurium-Containing Imidodiphosphinate Ligands:
 Preparation of Two Morphologies of Phase-Pure PbTe from a Single-Source
 Precursor
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1198
_journal_page_last               1205
_journal_paper_doi               10.1021/ic9021728
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C24 H56 N2 P4 Pb Se4'
_chemical_formula_sum            'C24 H56 N2 P4 Pb Se4'
_chemical_formula_weight         1019.63
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 117.14(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   32.019(6)
_cell_length_b                   9.4607(19)
_cell_length_c                   27.247(5)
_cell_measurement_reflns_used    38884
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.27
_cell_volume                     7345(3)
_computing_cell_refinement       'Nonius DENZO'
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'Nonius DENZO'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phiω scans'
_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  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            38884
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    8.750
_exptl_absorpt_correction_T_max  0.6218
_exptl_absorpt_correction_T_min  0.1788
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.844
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             3936
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.035
_refine_diff_density_min         -1.004
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         8391
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0306
_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)+(0.0240P)²+52.0374P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0744
_reflns_number_gt                7428
_reflns_number_total             8391
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9021728_si_002_1.cif
_cod_data_source_block           Compound4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4314719
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Pb1 Pb 0.084864(6) 0.331704(17) 0.305617(6) 0.02287(5) Uani 1 1 d . . .
Se2 Se 0.109361(18) 0.05901(5) 0.34647(2) 0.03283(11) Uani 1 1 d . . .
P2 P 0.16733(4) -0.02976(11) 0.33386(4) 0.0198(2) Uani 1 1 d . . .
C1 C 0.1139(2) -0.0411(6) 0.2209(2) 0.0425(13) Uani 1 1 d . . .
H1A H 0.1053 -0.0954 0.1870 0.064 Uiso 1 1 calc R . .
H1B H 0.1335 0.0395 0.2218 0.064 Uiso 1 1 calc R . .
H1C H 0.0855 -0.0068 0.2220 0.064 Uiso 1 1 calc R . .
C2 C 0.14140(16) -0.1357(5) 0.27091(18) 0.0264(9) Uani 1 1 d . . .
H2A H 0.1678 -0.1791 0.2661 0.032 Uiso 1 1 calc R . .
C3 C 0.11048(18) -0.2567(5) 0.2735(2) 0.0336(11) Uani 1 1 d . . .
H3A H 0.0978 -0.3103 0.2389 0.050 Uiso 1 1 calc R . .
H3B H 0.0846 -0.2176 0.2790 0.050 Uiso 1 1 calc R . .
H3C H 0.1294 -0.3196 0.3043 0.050 Uiso 1 1 calc R . .
C4 C 0.22110(18) -0.0715(5) 0.44567(18) 0.0325(10) Uani 1 1 d . . .
H4A H 0.2347 -0.1387 0.4763 0.049 Uiso 1 1 calc R . .
H4B H 0.1986 -0.0104 0.4507 0.049 Uiso 1 1 calc R . .
H4C H 0.2461 -0.0135 0.4448 0.049 Uiso 1 1 calc R . .
C5 C 0.19588(16) -0.1526(4) 0.39132(18) 0.0236(9) Uani 1 1 d . . .
H5A H 0.1709 -0.2119 0.3935 0.028 Uiso 1 1 calc R . .
C6 C 0.22995(18) -0.2520(5) 0.3827(2) 0.0335(11) Uani 1 1 d . . .
H6A H 0.2452 -0.3145 0.4147 0.050 Uiso 1 1 calc R . .
H6B H 0.2538 -0.1959 0.3783 0.050 Uiso 1 1 calc R . .
H6C H 0.2125 -0.3090 0.3494 0.050 Uiso 1 1 calc R . .
N1 N 0.20661(13) 0.0672(4) 0.33183(16) 0.0256(8) Uani 1 1 d . . .
P1 P 0.22290(4) 0.22202(11) 0.32643(4) 0.0182(2) Uani 1 1 d . . .
C7 C 0.2438(2) 0.3151(5) 0.4312(2) 0.0362(11) Uani 1 1 d . . .
H7A H 0.2679 0.3203 0.4697 0.054 Uiso 1 1 calc R . .
H7B H 0.2210 0.2414 0.4274 0.054 Uiso 1 1 calc R . .
H7C H 0.2277 0.4064 0.4201 0.054 Uiso 1 1 calc R . .
C8 C 0.26650(15) 0.2801(5) 0.39452(17) 0.0234(9) Uani 1 1 d . . .
H8A H 0.2883 0.1989 0.4119 0.028 Uiso 1 1 calc R . .
C9 C 0.29647(17) 0.4055(5) 0.3925(2) 0.0358(11) Uani 1 1 d . . .
H9A H 0.3173 0.4369 0.4301 0.054 Uiso 1 1 calc R . .
H9B H 0.2758 0.4836 0.3718 0.054 Uiso 1 1 calc R . .
H9C H 0.3153 0.3758 0.3743 0.054 Uiso 1 1 calc R . .
C10 C 0.2965(2) 0.1097(6) 0.3112(2) 0.0417(13) Uani 1 1 d . . .
H10A H 0.3122 0.1044 0.2877 0.062 Uiso 1 1 calc R . .
H10B H 0.2859 0.0152 0.3153 0.062 Uiso 1 1 calc R . .
H10C H 0.3184 0.1463 0.3476 0.062 Uiso 1 1 calc R . .
C11 C 0.25404(17) 0.2087(5) 0.28473(19) 0.0277(9) Uani 1 1 d . . .
H11A H 0.2659 0.3051 0.2824 0.033 Uiso 1 1 calc R . .
C12 C 0.2213(2) 0.1604(6) 0.2261(2) 0.0406(12) Uani 1 1 d . . .
H12A H 0.2385 0.1591 0.2042 0.061 Uiso 1 1 calc R . .
H12B H 0.1948 0.2258 0.2094 0.061 Uiso 1 1 calc R . .
H12C H 0.2097 0.0652 0.2272 0.061 Uiso 1 1 calc R . .
Se1 Se 0.170020(15) 0.38513(5) 0.289811(19) 0.02555(10) Uani 1 1 d . . .
Se4 Se 0.131983(15) 0.47474(5) 0.409887(18) 0.02435(9) Uani 1 1 d . . .
P4 P 0.07851(4) 0.57378(11) 0.42760(4) 0.0178(2) Uani 1 1 d . . .
C13 C 0.14486(17) 0.7707(5) 0.4965(2) 0.0318(10) Uani 1 1 d . . .
H13A H 0.1599 0.8144 0.5331 0.048 Uiso 1 1 calc R . .
H13B H 0.1276 0.8428 0.4688 0.048 Uiso 1 1 calc R . .
H13C H 0.1689 0.7284 0.4883 0.048 Uiso 1 1 calc R . .
C14 C 0.11098(15) 0.6565(4) 0.49545(17) 0.0225(8) Uani 1 1 d . . .
H14A H 0.0874 0.7031 0.5046 0.027 Uiso 1 1 calc R . .
C15 C 0.13659(17) 0.5456(5) 0.54015(18) 0.0318(10) Uani 1 1 d . . .
H15A H 0.1517 0.5919 0.5763 0.048 Uiso 1 1 calc R . .
H15B H 0.1604 0.4986 0.5328 0.048 Uiso 1 1 calc R . .
H15C H 0.1140 0.4755 0.5399 0.048 Uiso 1 1 calc R . .
C16 C 0.02373(18) 0.8218(5) 0.39693(19) 0.0303(10) Uani 1 1 d . . .
H16A H 0.0114 0.8997 0.3704 0.046 Uiso 1 1 calc R . .
H16B H 0.0441 0.8599 0.4336 0.046 Uiso 1 1 calc R . .
H16C H -0.0024 0.7701 0.3979 0.046 Uiso 1 1 calc R . .
C17 C 0.05223(15) 0.7208(5) 0.37931(16) 0.0220(8) Uani 1 1 d . . .
H17A H 0.0784 0.7765 0.3783 0.026 Uiso 1 1 calc R . .
C18 C 0.02143(17) 0.6664(5) 0.32124(18) 0.0308(10) Uani 1 1 d . . .
H18A H 0.0074 0.7466 0.2963 0.046 Uiso 1 1 calc R . .
H18B H -0.0035 0.6067 0.3214 0.046 Uiso 1 1 calc R . .
H18C H 0.0406 0.6109 0.3086 0.046 Uiso 1 1 calc R . .
N2 N 0.03895(12) 0.4797(4) 0.43152(14) 0.0203(7) Uani 1 1 d . . .
P3 P 0.01120(4) 0.33561(11) 0.40875(4) 0.0194(2) Uani 1 1 d . . .
C19 C -0.07277(17) 0.4830(6) 0.3618(2) 0.0361(11) Uani 1 1 d . . .
H19A H -0.1030 0.5028 0.3614 0.054 Uiso 1 1 calc R . .
H19B H -0.0781 0.4528 0.3250 0.054 Uiso 1 1 calc R . .
H19C H -0.0534 0.5687 0.3723 0.054 Uiso 1 1 calc R . .
C20 C -0.04764(15) 0.3663(5) 0.40315(19) 0.0274(9) Uani 1 1 d . . .
H20A H -0.0432 0.4003 0.4400 0.033 Uiso 1 1 calc R . .
C21 C -0.07706(19) 0.2311(6) 0.3900(2) 0.0417(13) Uani 1 1 d . . .
H21A H -0.1076 0.2524 0.3883 0.062 Uiso 1 1 calc R . .
H21B H -0.0607 0.1607 0.4189 0.062 Uiso 1 1 calc R . .
H21C H -0.0817 0.1935 0.3543 0.062 Uiso 1 1 calc R . .
C22 C 0.0351(2) 0.2331(6) 0.5145(2) 0.0405(13) Uani 1 1 d . . .
H22A H 0.0508 0.1591 0.5420 0.061 Uiso 1 1 calc R . .
H22B H 0.0023 0.2408 0.5073 0.061 Uiso 1 1 calc R . .
H22C H 0.0511 0.3236 0.5285 0.061 Uiso 1 1 calc R . .
C23 C 0.03713(17) 0.1957(5) 0.46111(18) 0.0266(9) Uani 1 1 d . . .
H23A H 0.0180 0.1081 0.4460 0.032 Uiso 1 1 calc R . .
C24 C 0.08709(18) 0.1626(5) 0.4719(2) 0.0339(11) Uani 1 1 d . . .
H24A H 0.0994 0.0844 0.4983 0.051 Uiso 1 1 calc R . .
H24B H 0.1068 0.2463 0.4872 0.051 Uiso 1 1 calc R . .
H24C H 0.0872 0.1357 0.4373 0.051 Uiso 1 1 calc R . .
Se3 Se 0.002868(15) 0.24908(5) 0.330681(17) 0.02518(10) Uani 1 1 d . . .
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'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 '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
Se2 Pb1 Se4 96.68(2) . . ?
Se2 Pb1 Se1 96.048(17) . . ?
Se4 Pb1 Se1 87.76(3) . . ?
Se2 Pb1 Se3 77.887(17) . . ?
Se4 Pb1 Se3 90.94(2) . . ?
Se1 Pb1 Se3 173.61(3) . . ?
Se2 Pb1 Se3 99.07(2) . 2 ?
Se4 Pb1 Se3 159.871(14) . 2 ?
Se1 Pb1 Se3 102.90(3) . 2 ?
Se3 Pb1 Se3 80.25(2) . 2 ?
P2 Se2 Pb1 113.31(3) . . ?
N1 P2 C5 107.7(2) . . ?
N1 P2 C2 108.3(2) . . ?
C5 P2 C2 106.9(2) . . ?
N1 P2 Se2 121.73(14) . . ?
C5 P2 Se2 103.70(15) . . ?
C2 P2 Se2 107.54(16) . . ?
C1 C2 C3 110.9(4) . . ?
C1 C2 P2 110.2(3) . . ?
C3 C2 P2 113.1(3) . . ?
C4 C5 C6 110.9(4) . . ?
C4 C5 P2 110.4(3) . . ?
C6 C5 P2 111.7(3) . . ?
P2 N1 P1 147.4(3) . . ?
N1 P1 C8 108.4(2) . . ?
N1 P1 C11 106.9(2) . . ?
C8 P1 C11 105.8(2) . . ?
N1 P1 Se1 118.68(15) . . ?
C8 P1 Se1 109.16(15) . . ?
C11 P1 Se1 107.22(16) . . ?
C7 C8 C9 110.4(4) . . ?
C7 C8 P1 111.1(3) . . ?
C9 C8 P1 113.3(3) . . ?
C12 C11 C10 110.3(4) . . ?
C12 C11 P1 111.3(3) . . ?
C10 C11 P1 111.5(3) . . ?
P1 Se1 Pb1 112.65(3) . . ?
P4 Se4 Pb1 107.97(4) . . ?
N2 P4 C14 105.89(19) . . ?
N2 P4 C17 110.7(2) . . ?
C14 P4 C17 105.3(2) . . ?
N2 P4 Se4 120.12(14) . . ?
C14 P4 Se4 105.32(15) . . ?
C17 P4 Se4 108.38(14) . . ?
C13 C14 C15 110.7(4) . . ?
C13 C14 P4 113.2(3) . . ?
C15 C14 P4 111.2(3) . . ?
C18 C17 C16 109.8(4) . . ?
C18 C17 P4 110.9(3) . . ?
C16 C17 P4 112.9(3) . . ?
P3 N2 P4 140.7(2) . . ?
N2 P3 C20 105.4(2) . . ?
N2 P3 C23 109.9(2) . . ?
C20 P3 C23 105.1(2) . . ?
N2 P3 Se3 120.04(13) . . ?
C20 P3 Se3 108.25(15) . . ?
C23 P3 Se3 107.29(15) . . ?
C19 C20 C21 111.8(4) . . ?
C19 C20 P3 110.6(3) . . ?
C21 C20 P3 112.6(3) . . ?
C24 C23 C22 111.1(4) . . ?
C24 C23 P3 111.1(3) . . ?
C22 C23 P3 111.8(3) . . ?
P3 Se3 Pb1 112.43(4) . . ?
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
Pb1 Se2 2.7773(7) . ?
Pb1 Se4 2.8754(9) . ?
Pb1 Se1 2.9911(7) . ?
Pb1 Se3 3.0994(7) . ?
Pb1 Se3 3.5742(15) 2 ?
Se2 P2 2.2023(12) . ?
P2 N1 1.578(4) . ?
P2 C5 1.825(4) . ?
P2 C2 1.827(5) . ?
C1 C2 1.528(7) . ?
C2 C3 1.537(6) . ?
C4 C5 1.530(6) . ?
C5 C6 1.538(6) . ?
N1 P1 1.584(4) . ?
P1 C8 1.825(4) . ?
P1 C11 1.826(4) . ?
P1 Se1 2.1684(12) . ?
C7 C8 1.517(6) . ?
C8 C9 1.543(7) . ?
C10 C11 1.533(7) . ?
C11 C12 1.526(7) . ?
Se4 P4 2.1901(11) . ?
P4 N2 1.591(3) . ?
P4 C14 1.832(4) . ?
P4 C17 1.834(4) . ?
C13 C14 1.522(6) . ?
C14 C15 1.531(6) . ?
C16 C17 1.542(6) . ?
C17 C18 1.522(6) . ?
N2 P3 1.590(4) . ?
P3 C20 1.842(5) . ?
P3 C23 1.843(5) . ?
P3 Se3 2.1791(12) . ?
C19 C20 1.519(7) . ?
C20 C21 1.531(7) . ?
C22 C23 1.526(6) . ?
C23 C24 1.521(7) . ?
