#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:18:03 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179054 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/16/4301690.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_4301690
loop_
_publ_author_name
'Jhon A. Balanta-Díaz'
'Mónica Moya-Cabrera'
'Vojtech Jancik'
'Leslie W. Pineda-Cedeño'
'Rubén A. Toscano'
'Raymundo Cea-Olivares'
_publ_section_title
;
Structural Variety of Alkali Metal Compounds Containing P-E-M (E = S,
Se; M = Li, Na, K) Units Derived from Nitrogen Rich Heterocycles
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2518
_journal_page_last               2525
_journal_paper_doi               10.1021/ic801950q
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C68 H72 N6 Na2 O4 P4 S4'
_chemical_formula_sum            'C68 H72 N6 Na2 O4 P4 S4'
_chemical_formula_weight         1335.42
_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                75.46(2)
_cell_angle_beta                 78.20(3)
_cell_angle_gamma                82.76(2)
_cell_formula_units_Z            1
_cell_length_a                   10.577(2)
_cell_length_b                   12.779(2)
_cell_length_c                   12.988(3)
_cell_measurement_reflns_used    9674
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.34
_cell_measurement_theta_min      2.33
_cell_volume                     1658.2(6)
_computing_cell_refinement       'Bruker AXS SAINT (v 7.01A, Bruker 2003)'
_computing_data_collection       'SMART V 5.625 (Bruker, 1999)'
_computing_data_reduction        'Bruker AXS SAINT (v 7.01A, Bruker 2003)'
_computing_molecular_graphics    'Bruker AXS SHELXTL (v 6.12)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 0.661
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Smart Apex CCD diffractometer'
_diffrn_measurement_method       'omega scan'
_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  0.0420
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20737
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    0.306
_exptl_absorpt_correction_T_max  0.9651
_exptl_absorpt_correction_T_min  0.9362
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs, Sheldrick 1996'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.210
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         5837
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0525P)²+0.5836P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1050
_reflns_number_gt                4973
_reflns_number_total             5837
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801950q_si_002_4.cif
_cod_data_source_block           Compound4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_database_code               4301690
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
O1 O 0.41080(17) 0.77432(14) -0.23599(15) 0.0396(4) Uani 1 1 d . . .
S1 S 0.25976(6) 0.52441(5) -0.27473(5) 0.02742(16) Uani 1 1 d . . .
P1 P 0.29983(5) 0.37119(5) -0.20841(5) 0.01947(14) Uani 1 1 d . . .
Na1 Na 0.46264(8) 0.58777(7) -0.17129(7) 0.0261(2) Uani 1 1 d . . .
N1 N 0.40078(17) 0.41176(15) -0.05350(15) 0.0218(4) Uani 1 1 d . . .
C1 C 0.3116(2) 0.35231(17) -0.06874(17) 0.0194(5) Uani 1 1 d . . .
P2 P 0.14398(5) 0.19040(4) 0.08124(5) 0.01966(15) Uani 1 1 d . . .
S2 S 0.21651(6) 0.05155(5) 0.04947(5) 0.02971(16) Uani 1 1 d . . .
N2 N 0.39890(18) 0.39085(15) 0.05294(15) 0.0244(4) Uani 1 1 d . . .
C2 C 0.2552(2) 0.29498(16) 0.03271(17) 0.0180(5) Uani 1 1 d . . .
O2 O 0.62729(16) 0.57749(14) -0.31827(14) 0.0375(4) Uani 1 1 d . . .
N3 N 0.31130(18) 0.32091(15) 0.10700(15) 0.0240(4) Uani 1 1 d . . .
C3 C 0.1850(2) 0.28431(18) -0.22304(17) 0.0213(5) Uani 1 1 d . . .
C4 C 0.2176(2) 0.17442(19) -0.21657(19) 0.0286(5) Uani 1 1 d . . .
H4A H 0.3007 0.1435 -0.2027 0.034 Uiso 1 1 calc R . .
C5 C 0.1296(3) 0.1097(2) -0.2303(2) 0.0340(6) Uani 1 1 d . . .
H5A H 0.1519 0.0344 -0.2251 0.041 Uiso 1 1 calc R . .
C6 C 0.0094(2) 0.1548(2) -0.2514(2) 0.0341(6) Uani 1 1 d . . .
H6A H -0.0514 0.1103 -0.2600 0.041 Uiso 1 1 calc R . .
C7 C -0.0230(2) 0.2642(2) -0.2600(2) 0.0331(6) Uani 1 1 d . . .
H7A H -0.1053 0.2951 -0.2759 0.040 Uiso 1 1 calc R . .
C8 C 0.0641(2) 0.3291(2) -0.24566(19) 0.0269(5) Uani 1 1 d . . .
H8A H 0.0413 0.4044 -0.2512 0.032 Uiso 1 1 calc R . .
C9 C 0.4562(2) 0.31644(18) -0.26852(18) 0.0228(5) Uani 1 1 d . . .
C10 C 0.5245(2) 0.22950(19) -0.2088(2) 0.0282(5) Uani 1 1 d . . .
H10A H 0.4926 0.2020 -0.1342 0.034 Uiso 1 1 calc R . .
C11 C 0.6387(2) 0.1836(2) -0.2586(2) 0.0364(6) Uani 1 1 d . . .
H11A H 0.6851 0.1245 -0.2180 0.044 Uiso 1 1 calc R . .
C12 C 0.6852(2) 0.2229(2) -0.3661(2) 0.0391(7) Uani 1 1 d . . .
H12A H 0.7630 0.1902 -0.3999 0.047 Uiso 1 1 calc R . .
C13 C 0.6201(2) 0.3097(2) -0.4256(2) 0.0390(7) Uani 1 1 d . . .
H13A H 0.6537 0.3372 -0.4999 0.047 Uiso 1 1 calc R . .
C14 C 0.5052(2) 0.3570(2) -0.3769(2) 0.0313(6) Uani 1 1 d . . .
H14A H 0.4605 0.4171 -0.4178 0.038 Uiso 1 1 calc R . .
C15 C 0.1020(2) 0.18214(18) 0.22607(18) 0.0233(5) Uani 1 1 d . . .
C16 C 0.1552(2) 0.0952(2) 0.2963(2) 0.0312(6) Uani 1 1 d . . .
H16A H 0.2138 0.0421 0.2684 0.037 Uiso 1 1 calc R . .
C17 C 0.1233(3) 0.0857(2) 0.4069(2) 0.0394(7) Uani 1 1 d . . .
H17A H 0.1606 0.0264 0.4546 0.047 Uiso 1 1 calc R . .
C18 C 0.0372(3) 0.1621(2) 0.4478(2) 0.0417(7) Uani 1 1 d . . .
H18A H 0.0146 0.1550 0.5238 0.050 Uiso 1 1 calc R . .
C19 C -0.0157(2) 0.2481(2) 0.3790(2) 0.0395(7) Uani 1 1 d . . .
H19A H -0.0748 0.3007 0.4074 0.047 Uiso 1 1 calc R . .
C20 C 0.0166(2) 0.2588(2) 0.2685(2) 0.0310(6) Uani 1 1 d . . .
H20A H -0.0199 0.3190 0.2213 0.037 Uiso 1 1 calc R . .
C21 C -0.0046(2) 0.24461(18) 0.03117(17) 0.0209(5) Uani 1 1 d . . .
C22 C -0.0882(2) 0.17515(19) 0.01942(18) 0.0242(5) Uani 1 1 d . . .
H22A H -0.0641 0.0995 0.0313 0.029 Uiso 1 1 calc R . .
C23 C -0.2065(2) 0.2154(2) -0.00957(19) 0.0296(6) Uani 1 1 d . . .
H23A H -0.2639 0.1673 -0.0169 0.036 Uiso 1 1 calc R . .
C24 C -0.2418(2) 0.3258(2) -0.02801(19) 0.0301(6) Uani 1 1 d . . .
H24A H -0.3236 0.3533 -0.0473 0.036 Uiso 1 1 calc R . .
C25 C -0.1575(2) 0.39589(19) -0.0182(2) 0.0294(6) Uani 1 1 d . . .
H25A H -0.1810 0.4717 -0.0320 0.035 Uiso 1 1 calc R . .
C26 C -0.0393(2) 0.35579(19) 0.01145(19) 0.0257(5) Uani 1 1 d . . .
H26A H 0.0182 0.4040 0.0184 0.031 Uiso 1 1 calc R . .
C27 C 0.3150(3) 0.8181(2) -0.3008(2) 0.0441(7) Uani 1 1 d . . .
H27A H 0.2333 0.8397 -0.2557 0.053 Uiso 1 1 calc R . .
H27B H 0.2972 0.7639 -0.3377 0.053 Uiso 1 1 calc R . .
C28 C 0.3693(3) 0.9155(2) -0.3823(2) 0.0524(8) Uani 1 1 d . . .
H28A H 0.3017 0.9764 -0.3921 0.063 Uiso 1 1 calc R . .
H28B H 0.4046 0.8976 -0.4530 0.063 Uiso 1 1 calc R . .
C29 C 0.4760(3) 0.9442(2) -0.3345(3) 0.0560(8) Uani 1 1 d . . .
H29A H 0.5618 0.9344 -0.3801 0.067 Uiso 1 1 calc R . .
H29B H 0.4613 1.0202 -0.3268 0.067 Uiso 1 1 calc R . .
C30 C 0.4670(3) 0.8662(2) -0.2258(3) 0.0504(8) Uani 1 1 d . . .
H30A H 0.5541 0.8450 -0.2067 0.060 Uiso 1 1 calc R . .
H30B H 0.4119 0.8993 -0.1692 0.060 Uiso 1 1 calc R . .
C31 C 0.7400(3) 0.5076(2) -0.3016(2) 0.0474(7) Uani 1 1 d . . .
H31A H 0.7181 0.4311 -0.2776 0.057 Uiso 1 1 calc R . .
H31B H 0.7793 0.5249 -0.2455 0.057 Uiso 1 1 calc R . .
C32 C 0.8337(3) 0.5250(3) -0.4089(3) 0.0566(8) Uani 1 1 d . . .
H32A H 0.9216 0.5347 -0.3992 0.068 Uiso 1 1 calc R . .
H32B H 0.8386 0.4629 -0.4427 0.068 Uiso 1 1 calc R . .
C33 C 0.7765(3) 0.6275(3) -0.4770(2) 0.0490(8) Uani 1 1 d . . .
H33A H 0.7396 0.6111 -0.5348 0.059 Uiso 1 1 calc R . .
H33B H 0.8428 0.6802 -0.5103 0.059 Uiso 1 1 calc R . .
C34 C 0.6713(3) 0.6708(2) -0.3962(2) 0.0464(7) Uani 1 1 d . . .
H34A H 0.7066 0.7192 -0.3622 0.056 Uiso 1 1 calc R . .
H34B H 0.5999 0.7116 -0.4318 0.056 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'
Na Na 0.0362 0.0249 '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'
S S 0.1246 0.1234 '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
C27 O1 C30 105.0(2) . . ?
C27 O1 Na1 124.62(16) . . ?
C30 O1 Na1 130.33(16) . . ?
P1 S1 Na1 89.96(4) . . ?
C1 P1 C3 110.84(10) . . ?
C1 P1 C9 103.85(10) . . ?
C3 P1 C9 104.57(10) . . ?
C1 P1 S1 111.28(8) . . ?
C3 P1 S1 112.47(8) . . ?
C9 P1 S1 113.33(8) . . ?
O2 Na1 O1 93.47(7) . . ?
O2 Na1 N2 96.04(7) . 2_665 ?
O1 Na1 N2 95.90(7) . 2_665 ?
O2 Na1 N1 115.01(7) . . ?
O1 Na1 N1 149.59(7) . . ?
N2 Na1 N1 91.64(7) 2_665 . ?
O2 Na1 S1 93.38(6) . . ?
O1 Na1 S1 92.62(6) . . ?
N2 Na1 S1 166.87(6) 2_665 . ?
N1 Na1 S1 76.07(5) . . ?
N2 N1 C1 107.15(17) . . ?
N2 N1 Na1 120.74(13) . . ?
C1 N1 Na1 124.79(15) . . ?
N1 C1 C2 107.22(19) . . ?
N1 C1 P1 113.36(16) . . ?
C2 C1 P1 139.41(17) . . ?
C2 P2 C21 107.05(10) . . ?
C2 P2 C15 103.81(10) . . ?
C21 P2 C15 104.32(10) . . ?
C2 P2 S2 113.49(8) . . ?
C21 P2 S2 115.09(8) . . ?
C15 P2 S2 112.08(8) . . ?
N3 N2 N1 111.02(17) . . ?
N3 N2 Na1 109.94(13) . 2_665 ?
N1 N2 Na1 137.38(14) . 2_665 ?
N3 C2 C1 107.57(18) . . ?
N3 C2 P2 117.04(16) . . ?
C1 C2 P2 135.01(17) . . ?
C34 O2 C31 105.5(2) . . ?
C34 O2 Na1 122.33(16) . . ?
C31 O2 Na1 119.01(16) . . ?
N2 N3 C2 107.04(18) . . ?
C4 C3 C8 119.3(2) . . ?
C4 C3 P1 121.13(17) . . ?
C8 C3 P1 119.53(17) . . ?
C5 C4 C3 120.3(2) . . ?
C6 C5 C4 119.9(2) . . ?
C5 C6 C7 120.3(2) . . ?
C6 C7 C8 120.2(2) . . ?
C7 C8 C3 120.1(2) . . ?
C14 C9 C10 119.4(2) . . ?
C14 C9 P1 119.64(18) . . ?
C10 C9 P1 120.89(18) . . ?
C11 C10 C9 119.9(2) . . ?
C12 C11 C10 120.4(2) . . ?
C11 C12 C13 120.4(2) . . ?
C12 C13 C14 120.1(2) . . ?
C9 C14 C13 119.9(2) . . ?
C20 C15 C16 119.0(2) . . ?
C20 C15 P2 122.09(18) . . ?
C16 C15 P2 118.94(19) . . ?
C17 C16 C15 120.3(2) . . ?
C18 C17 C16 120.0(3) . . ?
C19 C18 C17 120.0(2) . . ?
C18 C19 C20 120.3(3) . . ?
C19 C20 C15 120.4(2) . . ?
C22 C21 C26 119.7(2) . . ?
C22 C21 P2 120.09(17) . . ?
C26 C21 P2 120.12(17) . . ?
C23 C22 C21 120.2(2) . . ?
C22 C23 C24 120.2(2) . . ?
C25 C24 C23 119.8(2) . . ?
C26 C25 C24 120.1(2) . . ?
C25 C26 C21 120.0(2) . . ?
O1 C27 C28 106.2(2) . . ?
C27 C28 C29 104.6(2) . . ?
C30 C29 C28 103.8(2) . . ?
O1 C30 C29 105.6(2) . . ?
O2 C31 C32 107.1(2) . . ?
C33 C32 C31 104.0(2) . . ?
C32 C33 C34 103.5(2) . . ?
O2 C34 C33 104.9(2) . . ?
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
O1 C27 1.420(3) . ?
O1 C30 1.427(3) . ?
O1 Na1 2.354(2) . ?
S1 P1 1.9618(9) . ?
S1 Na1 3.0379(12) . ?
P1 C1 1.797(2) . ?
P1 C3 1.812(2) . ?
P1 C9 1.813(2) . ?
Na1 O2 2.324(2) . ?
Na1 N2 2.411(2) 2_665 ?
Na1 N1 2.462(2) . ?
N1 N2 1.337(3) . ?
N1 C1 1.356(3) . ?
C1 C2 1.390(3) . ?
P2 C2 1.799(2) . ?
P2 C21 1.814(2) . ?
P2 C15 1.821(2) . ?
P2 S2 1.9499(9) . ?
N2 N3 1.333(3) . ?
N2 Na1 2.411(2) 2_665 ?
C2 N3 1.355(3) . ?
O2 C34 1.415(3) . ?
O2 C31 1.416(3) . ?
C3 C4 1.389(3) . ?
C3 C8 1.391(3) . ?
C4 C5 1.385(3) . ?
C5 C6 1.379(4) . ?
C6 C7 1.379(4) . ?
C7 C8 1.382(3) . ?
C9 C14 1.386(3) . ?
C9 C10 1.397(3) . ?
C10 C11 1.383(3) . ?
C11 C12 1.369(4) . ?
C12 C13 1.376(4) . ?
C13 C14 1.391(4) . ?
C15 C20 1.387(3) . ?
C15 C16 1.388(3) . ?
C16 C17 1.384(4) . ?
C17 C18 1.379(4) . ?
C18 C19 1.370(4) . ?
C19 C20 1.381(3) . ?
C21 C22 1.384(3) . ?
C21 C26 1.394(3) . ?
C22 C23 1.380(3) . ?
C23 C24 1.386(3) . ?
C24 C25 1.385(3) . ?
C25 C26 1.382(3) . ?
C27 C28 1.506(4) . ?
C28 C29 1.516(4) . ?
C29 C30 1.502(4) . ?
C31 C32 1.520(4) . ?
C32 C33 1.517(4) . ?
C33 C34 1.518(4) . ?
