#------------------------------------------------------------------------------
#$Date: 2017-10-04 18:10:59 +0300 (Wed, 04 Oct 2017) $
#$Revision: 201626 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/65/4126534.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_4126534
loop_
_publ_author_name
'Hennersdorf, Felix'
'Frötschel, Julia'
'Weigand, Jan J.'
_publ_section_title
;
 Selective Derivatization of a Hexaphosphane from Functionalization of
 White Phosphorus.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b07704
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         '0.25(C48 H96 Na4 O24), C O P'
_chemical_formula_sum            'C13 H24 Na O7 P'
_chemical_formula_weight         346.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-06-21
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.4915(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.74960(8)
_cell_length_b                   10.45685(7)
_cell_length_c                   14.96661(11)
_cell_measurement_reflns_used    13487
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.0800
_cell_measurement_theta_min      4.1310
_cell_volume                     1671.56(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5700
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -96.00  46.00   0.50    1.00    --  -38.16  19.00 -90.00  284
  2  ω    -69.00  41.00   0.50    1.00    --  -38.16  38.00-180.00  220
  3  ω      6.00 116.00   0.50    1.00    --   38.16  57.00  90.00  220
  4  ω     23.00  97.00   0.50    1.00    --   38.16-125.00-180.00  148
  5  ω    100.00 178.00   0.50    4.00    --  115.00 111.00 -60.00  156
  6  ω     37.00 148.00   0.50    4.00    --  115.00 -61.00 150.00  222
  7  ω     28.00 109.00   0.50    4.00    --  115.00 -94.00 -60.00  162
  8  ω     84.00 178.00   0.50    4.00    --  115.00  45.00  30.00  188
  9  ω     82.00 178.00   0.50    4.00    --  115.00  61.00 -60.00  192
 10  ω    100.00 178.00   0.50    4.00    --  115.00 111.00 150.00  156
 11  ω     84.00 178.00   0.50    4.00    --  115.00  45.00 -90.00  188
 12  ω     60.00 107.00   0.50    4.00    --  115.00 -94.00  60.00   94
 13  ω    101.00 178.00   0.50    4.00    --  115.00 111.00  90.00  154
 14  ω     71.00  98.00   0.50    4.00    --  115.00 178.00 -60.00   54
 15  ω    107.00 177.00   0.50    4.00    --  115.00  30.00   0.00  140
 16  ω   -122.00 -85.00   0.50    1.00    --  -38.16 -19.00-120.00   74
 17  ω    -28.00  16.00   0.50    1.00    --  -38.16 -19.00-120.00   88
 18  ω     20.00  82.00   0.50    1.00    --   38.16 -99.00-150.00  124
 19  ω     26.00  52.00   0.50    1.00    --   38.16  38.00-180.00   52
 20  ω     91.00 117.00   0.50    1.00    --   38.16  38.00-180.00   52
 21  ω     69.00  95.00   0.50    1.00    --   38.16  19.00   0.00   52
 22  ω     30.00  69.00   0.50    1.00    --   38.16  38.00  60.00   78
 23  ω     30.00  82.00   0.50    1.00    --   38.16-125.00  30.00  104
 24  ω     74.00 102.00   0.50    4.00    --  115.00 -94.00-120.00   56
 25  ω     80.00 106.00   0.50    4.00    --  115.00  77.00  30.00   52
 26  ω     38.00  71.00   0.50    4.00    --  115.00 -94.00-120.00   66
 27  ω     71.00  97.00   0.50    4.00    --  115.00 178.00 150.00   52
 28  ω     79.00 104.00   0.50    4.00    --  115.00  77.00   0.00   50
 29  ω     86.00 112.00   0.50    4.00    --  115.00  30.00  30.00   52
 30  ω     79.00 105.00   0.50    4.00    --  115.00  77.00 -30.00   52
 31  ω     82.00 107.00   0.50    4.00    --  115.00  61.00   0.00   50
 32  ω     82.00 114.00   0.50    4.00    --  115.00  77.00  60.00   64
 33  ω     29.00  95.00   0.50    4.00    --  115.00 -94.00 120.00  132
 34  ω     42.00  80.00   0.50    4.00    --  115.00 -94.00 150.00   76
 35  ω    153.00 178.00   0.50    4.00    --  115.00  77.00  60.00   50
 36  ω     84.00 110.00   0.50    4.00    --  115.00  45.00   0.00   52
 37  ω     86.00 112.00   0.50    4.00    --  115.00  45.00  60.00   52
 38  ω     85.00 110.00   0.50    4.00    --  115.00  61.00 -30.00   50
 39  ω     87.00 113.00   0.50    4.00    --  115.00  45.00 -30.00   52
 40  ω     50.00  76.00   0.50    4.00    --  115.00  15.00  30.00   52
 41  ω    126.00 151.00   0.50    4.00    --  115.00 178.00 150.00   50
 42  ω     82.00 119.00   0.50    4.00    --  115.00  30.00  90.00   74
 43  ω     57.00  97.00   0.50    4.00    --  115.00 178.00 120.00   80
 44  ω     82.00 108.00   0.50    4.00    --  115.00  61.00  30.00   52
 45  ω     85.00 111.00   0.50    4.00    --  115.00  30.00  60.00   52
 46  ω    153.00 178.00   0.50    4.00    --  115.00  77.00 -30.00   50
 47  ω     36.00  61.00   0.50    4.00    --  115.00  15.00  60.00   50
 48  ω     82.00 107.00   0.50    4.00    --  115.00  61.00  60.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1188688000
_diffrn_orient_matrix_UB_12      0.0829976000
_diffrn_orient_matrix_UB_13      0.0150407000
_diffrn_orient_matrix_UB_21      -0.0141808000
_diffrn_orient_matrix_UB_22      0.0342554000
_diffrn_orient_matrix_UB_23      -0.1007444000
_diffrn_orient_matrix_UB_31      -0.0803411000
_diffrn_orient_matrix_UB_32      0.1168786000
_diffrn_orient_matrix_UB_33      0.0189404000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19621
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.288
_diffrn_reflns_theta_min         4.139
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.994
_exptl_absorpt_correction_T_max  0.845
_exptl_absorpt_correction_T_min  0.801
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_description       block
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.147
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.123
_refine_diff_density_max         0.249
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.46(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         5715
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0304
_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)+(0.0542P)²+0.2867P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0827
_reflns_Friedel_coverage         0.996
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                5635
_reflns_number_total             5715
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja7b07704_si_032.cif
_cod_data_source_block           NaOCP_2
_cod_original_cell_volume        1671.57(2)
_cod_database_code               4126534
_chemical_oxdiff_formula         'C13 H24 Na1 O7 P1'
_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.
;
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     51.96
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.54(2) 0.46(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
3. Uiso/Uaniso restraints and constraints
P2B \\sim O2B \\sim C2B: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Same fragment restrains
{P2B, O2B, C2B} sigma for 1-2: 0.02, 1-3: 0.02
as
{P2A, O2A, C2A}
5. Others
 Sof(P2B)=Sof(O2B)=Sof(C2B)=1-FVAR(1)
 Sof(P2A)=Sof(O2A)=Sof(C2A)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B),
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B),
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B),
  C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,
 H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.176
_oxdiff_exptl_absorpt_empirical_full_min 0.838
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Na1 Na 0.88609(8) 0.50174(7) 0.48452(6) 0.00986(16) Uani 1 1 d . . . . .
Na2 Na 0.38852(8) 0.99714(8) 0.52376(6) 0.00997(17) Uani 1 1 d . . . . .
O3 O 0.91420(17) 0.52043(15) 0.64408(11) 0.0171(3) Uani 1 1 d . . . . .
O4 O 0.85996(16) 0.50313(15) 0.82559(11) 0.0162(3) Uani 1 1 d . . . . .
O5 O 1.03489(15) 0.66908(15) 0.47297(11) 0.0168(3) Uani 1 1 d . . . . .
O6 O 1.25350(15) 0.81438(15) 0.52881(11) 0.0161(3) Uani 1 1 d . . . . .
O7 O 0.73325(16) 0.66311(15) 0.48724(11) 0.0158(3) Uani 1 1 d . . . . .
O8 O 0.55052(15) 0.84916(15) 0.51659(11) 0.0155(3) Uani 1 1 d . . . . .
O9 O 0.53485(15) 1.17461(15) 0.53054(11) 0.0151(3) Uani 1 1 d . . . . .
O10 O 0.73519(15) 1.33196(14) 0.48471(11) 0.0150(3) Uani 1 1 d . . . . .
O11 O 0.35897(17) 0.99607(15) 0.36507(12) 0.0170(3) Uani 1 1 d . . . . .
O12 O 0.41149(16) 1.01446(16) 0.18346(11) 0.0172(3) Uani 1 1 d . . . . .
O13 O 0.22206(15) 1.14382(15) 0.51772(11) 0.0146(3) Uani 1 1 d . . . . .
O14 O 0.04471(15) 1.34595(14) 0.49525(11) 0.0149(3) Uani 1 1 d . . . . .
C3 C 0.9628(2) 0.4184(2) 0.70285(16) 0.0175(4) Uani 1 1 d . . . . .
H3A H 1.0444 0.4422 0.7324 0.021 Uiso 1 1 calc R . . . .
H3B H 0.9726 0.3418 0.6678 0.021 Uiso 1 1 calc R . . . .
C4 C 0.8756(2) 0.3914(2) 0.77242(16) 0.0174(4) Uani 1 1 d . . . . .
H4A H 0.7949 0.3645 0.7429 0.021 Uiso 1 1 calc R . . . .
H4B H 0.9092 0.3223 0.8112 0.021 Uiso 1 1 calc R . . . .
C5 C 0.8989(2) 0.6325(2) 0.69735(15) 0.0169(4) Uani 1 1 d . . . . .
H5A H 0.8651 0.7015 0.6587 0.020 Uiso 1 1 calc R . . . .
H5B H 0.9798 0.6594 0.7267 0.020 Uiso 1 1 calc R . . . .
C6 C 0.8115(2) 0.6050(2) 0.76767(15) 0.0168(4) Uani 1 1 d . . . . .
H6A H 0.8020 0.6814 0.8031 0.020 Uiso 1 1 calc R . . . .
H6B H 0.7296 0.5815 0.7383 0.020 Uiso 1 1 calc R . . . .
C7 C 1.1443(2) 0.6609(2) 0.42638(16) 0.0173(4) Uani 1 1 d . . . . .
H7A H 1.1374 0.7217 0.3771 0.021 Uiso 1 1 calc R . . . .
H7B H 1.1502 0.5758 0.4014 0.021 Uiso 1 1 calc R . . . .
C8 C 1.2610(2) 0.6892(2) 0.48977(16) 0.0175(4) Uani 1 1 d . . . . .
H8A H 1.2704 0.6255 0.5371 0.021 Uiso 1 1 calc R . . . .
H8B H 1.3339 0.6847 0.4571 0.021 Uiso 1 1 calc R . . . .
C9 C 1.0276(2) 0.7946(2) 0.51081(16) 0.0170(4) Uani 1 1 d . . . . .
H9A H 0.9540 0.8005 0.5426 0.020 Uiso 1 1 calc R . . . .
H9B H 1.0198 0.8577 0.4630 0.020 Uiso 1 1 calc R . . . .
C10 C 1.1436(2) 0.8222(2) 0.57510(15) 0.0172(4) Uani 1 1 d . . . . .
H10A H 1.1375 0.9071 0.6004 0.021 Uiso 1 1 calc R . . . .
H10B H 1.1498 0.7609 0.6240 0.021 Uiso 1 1 calc R . . . .
C11 C 0.7033(2) 0.7657(2) 0.42428(16) 0.0165(4) Uani 1 1 d . . . . .
H11A H 0.6386 0.7381 0.3778 0.020 Uiso 1 1 calc R . . . .
H11B H 0.7769 0.7885 0.3958 0.020 Uiso 1 1 calc R . . . .
C12 C 0.6580(2) 0.8808(2) 0.47263(16) 0.0158(4) Uani 1 1 d . . . . .
H12A H 0.7245 0.9111 0.5168 0.019 Uiso 1 1 calc R . . . .
H12B H 0.6368 0.9491 0.4297 0.019 Uiso 1 1 calc R . . . .
C13 C 0.6258(2) 0.6320(2) 0.53124(16) 0.0160(4) Uani 1 1 d . . . . .
H13A H 0.6468 0.5640 0.5744 0.019 Uiso 1 1 calc R . . . .
H13B H 0.5593 0.6014 0.4872 0.019 Uiso 1 1 calc R . . . .
C14 C 0.5802(2) 0.7473(2) 0.57921(16) 0.0165(4) Uani 1 1 d . . . . .
H14A H 0.5065 0.7246 0.6075 0.020 Uiso 1 1 calc R . . . .
H14B H 0.6446 0.7751 0.6258 0.020 Uiso 1 1 calc R . . . .
C15 C 0.6534(2) 1.1788(2) 0.58531(15) 0.0161(4) Uani 1 1 d . . . . .
H15A H 0.6700 1.0965 0.6142 0.019 Uiso 1 1 calc R . . . .
H15B H 0.6505 1.2427 0.6320 0.019 Uiso 1 1 calc R . . . .
C16 C 0.7579(2) 1.2108(2) 0.52923(17) 0.0168(4) Uani 1 1 d . . . . .
H16A H 0.8368 1.2141 0.5676 0.020 Uiso 1 1 calc R . . . .
H16B H 0.7639 1.1444 0.4847 0.020 Uiso 1 1 calc R . . . .
C17 C 0.5125(2) 1.2955(2) 0.48546(16) 0.0155(4) Uani 1 1 d . . . . .
H17A H 0.5071 1.3626 0.5296 0.019 Uiso 1 1 calc R . . . .
H17B H 0.4334 1.2923 0.4472 0.019 Uiso 1 1 calc R . . . .
C18 C 0.6171(2) 1.3256(2) 0.42907(15) 0.0160(4) Uani 1 1 d . . . . .
H18A H 0.6208 1.2599 0.3837 0.019 Uiso 1 1 calc R . . . .
H18B H 0.6005 1.4068 0.3987 0.019 Uiso 1 1 calc R . . . .
C19 C 0.3749(2) 0.8845(2) 0.31181(15) 0.0171(4) Uani 1 1 d . . . . .
H19A H 0.2941 0.8568 0.2830 0.020 Uiso 1 1 calc R . . . .
H19B H 0.4098 0.8159 0.3504 0.020 Uiso 1 1 calc R . . . .
C20 C 0.4610(2) 0.9122(2) 0.24089(16) 0.0177(4) Uani 1 1 d . . . . .
H20A H 0.5432 0.9357 0.2697 0.021 Uiso 1 1 calc R . . . .
H20B H 0.4699 0.8360 0.2052 0.021 Uiso 1 1 calc R . . . .
C21 C 0.3103(2) 1.0982(2) 0.30762(15) 0.0164(4) Uani 1 1 d . . . . .
H21A H 0.3010 1.1743 0.3433 0.020 Uiso 1 1 calc R . . . .
H21B H 0.2283 1.0748 0.2783 0.020 Uiso 1 1 calc R . . . .
C22 C 0.3973(2) 1.1260(2) 0.23728(16) 0.0168(4) Uani 1 1 d . . . . .
H22A H 0.3637 1.1956 0.1991 0.020 Uiso 1 1 calc R . . . .
H22B H 0.4785 1.1521 0.2665 0.020 Uiso 1 1 calc R . . . .
C23 C 0.0995(2) 1.1249(2) 0.47052(15) 0.0151(4) Uani 1 1 d . . . . .
H23A H 0.0433 1.0940 0.5121 0.018 Uiso 1 1 calc R . . . .
H23B H 0.1036 1.0607 0.4242 0.018 Uiso 1 1 calc R . . . .
C24 C 0.0489(2) 1.2485(2) 0.42794(15) 0.0147(4) Uani 1 1 d . . . . .
H24A H 0.1019 1.2765 0.3834 0.018 Uiso 1 1 calc R . . . .
H24B H -0.0346 1.2343 0.3977 0.018 Uiso 1 1 calc R . . . .
C25 C 0.2168(2) 1.2413(2) 0.58480(15) 0.0164(4) Uani 1 1 d . . . . .
H25A H 0.2999 1.2552 0.6159 0.020 Uiso 1 1 calc R . . . .
H25B H 0.1625 1.2137 0.6286 0.020 Uiso 1 1 calc R . . . .
C26 C 0.1677(2) 1.3647(2) 0.54156(16) 0.0152(4) Uani 1 1 d . . . . .
H26A H 0.1646 1.4299 0.5874 0.018 Uiso 1 1 calc R . . . .
H26B H 0.2237 1.3940 0.4994 0.018 Uiso 1 1 calc R . . . .
P1 P 0.95456(9) 1.03405(7) 0.73002(7) 0.03384(18) Uani 1 1 d . . . . .
O1 O 0.7533(3) 0.9266(3) 0.8067(2) 0.0624(9) Uani 1 1 d . . . . .
C1 C 0.8360(3) 0.9718(2) 0.77394(18) 0.0212(5) Uani 1 1 d . . . . .
P2A P 0.45016(12) 0.53780(13) 0.23116(11) 0.0310(3) Uani 0.841(4) 1 d D . P A 1
O2A O 0.2494(3) 0.4103(3) 0.2934(3) 0.0809(15) Uani 0.841(4) 1 d D . P A 1
C2A C 0.3279(6) 0.4632(6) 0.2648(6) 0.0227(13) Uani 0.841(4) 1 d D . P A 1
P2B P 0.3291(11) 0.4754(12) 0.2816(8) 0.029(3) Uiso 0.159(4) 1 d D U P A 2
O2B O 0.5288(16) 0.5757(16) 0.2070(12) 0.052(4) Uiso 0.159(4) 1 d D U P A 2
C2B C 0.456(4) 0.519(5) 0.241(4) 0.074(16) Uiso 0.159(4) 1 d D U P A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.0616
-5 -4 2 0.0569
0 0 1 0.0616
4 -5 -2 0.0621
-4 5 2 0.0621
4 -5 4 0.0574
5 2 -3 0.0605
0 3 -5 0.0873
-4 5 5 0.0600
-2 -4 -5 0.0636
1 -2 -5 0.0632
5 2 5 0.0397
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
O3 Na1 O5 90.13(6) . .
O3 Na1 O10 93.93(7) . 1_545
O4 Na1 O3 176.49(7) 2_564 .
O4 Na1 O5 86.98(6) 2_564 .
O4 Na1 O10 88.97(6) 2_564 1_545
O5 Na1 O10 175.94(7) . 1_545
O7 Na1 O3 86.20(6) . .
O7 Na1 O4 91.66(6) . 2_564
O7 Na1 O5 87.17(6) . .
O7 Na1 O10 93.26(7) . 1_545
O14 Na1 O3 88.82(6) 1_645 .
O14 Na1 O4 93.24(6) 1_645 2_564
O14 Na1 O5 91.50(6) 1_645 .
O14 Na1 O7 174.84(7) 1_645 .
O14 Na1 O10 88.42(6) 1_645 1_545
O6 Na2 O9 175.03(7) 1_455 .
O8 Na2 O6 86.04(6) . 1_455
O8 Na2 O9 91.45(7) . .
O8 Na2 O11 88.11(7) . .
O8 Na2 O12 91.09(6) . 2_575
O8 Na2 O13 175.16(7) . .
O11 Na2 O6 90.85(7) . 1_455
O11 Na2 O9 93.36(7) . .
O11 Na2 O12 176.35(7) . 2_575
O12 Na2 O6 85.55(6) 2_575 1_455
O12 Na2 O9 90.22(6) 2_575 .
O13 Na2 O6 93.45(7) . 1_455
O13 Na2 O9 89.41(6) . .
O13 Na2 O11 87.09(6) . .
O13 Na2 O12 93.67(7) . 2_575
C3 O3 Na1 123.15(13) . .
C5 O3 Na1 127.87(13) . .
C5 O3 C3 108.73(17) . .
C4 O4 Na1 122.19(13) . 2_565
C6 O4 Na1 128.17(13) . 2_565
C6 O4 C4 109.11(17) . .
C7 O5 Na1 125.68(13) . .
C9 O5 Na1 125.03(13) . .
C9 O5 C7 109.29(16) . .
C8 O6 Na2 130.38(13) . 1_655
C10 O6 Na2 120.09(13) . 1_655
C10 O6 C8 109.52(16) . .
C11 O7 Na1 128.79(14) . .
C13 O7 Na1 116.48(12) . .
C13 O7 C11 109.73(17) . .
C12 O8 Na2 120.75(13) . .
C14 O8 Na2 125.03(14) . .
C14 O8 C12 109.97(17) . .
C15 O9 Na2 125.19(12) . .
C15 O9 C17 109.33(16) . .
C17 O9 Na2 125.33(13) . .
C16 O10 Na1 124.84(14) . 1_565
C18 O10 Na1 125.75(13) . 1_565
C18 O10 C16 108.64(17) . .
C19 O11 Na2 123.53(13) . .
C21 O11 Na2 126.80(13) . .
C21 O11 C19 109.33(17) . .
C20 O12 Na2 123.58(14) . 2_574
C22 O12 Na2 126.87(13) . 2_574
C22 O12 C20 108.94(18) . .
C23 O13 Na2 125.51(12) . .
C25 O13 Na2 121.74(13) . .
C25 O13 C23 109.59(17) . .
C24 O14 Na1 121.54(13) . 1_465
C26 O14 Na1 124.03(12) . 1_465
C26 O14 C24 109.62(17) . .
O3 C3 H3A 109.6 . .
O3 C3 H3B 109.6 . .
O3 C3 C4 110.49(19) . .
H3A C3 H3B 108.1 . .
C4 C3 H3A 109.6 . .
C4 C3 H3B 109.6 . .
O4 C4 C3 110.65(18) . .
O4 C4 H4A 109.5 . .
O4 C4 H4B 109.5 . .
C3 C4 H4A 109.5 . .
C3 C4 H4B 109.5 . .
H4A C4 H4B 108.1 . .
O3 C5 H5A 109.6 . .
O3 C5 H5B 109.6 . .
O3 C5 C6 110.46(18) . .
H5A C5 H5B 108.1 . .
C6 C5 H5A 109.6 . .
C6 C5 H5B 109.6 . .
O4 C6 C5 110.42(19) . .
O4 C6 H6A 109.6 . .
O4 C6 H6B 109.6 . .
C5 C6 H6A 109.6 . .
C5 C6 H6B 109.6 . .
H6A C6 H6B 108.1 . .
O5 C7 H7A 109.6 . .
O5 C7 H7B 109.6 . .
O5 C7 C8 110.50(19) . .
H7A C7 H7B 108.1 . .
C8 C7 H7A 109.6 . .
C8 C7 H7B 109.6 . .
O6 C8 C7 110.59(19) . .
O6 C8 H8A 109.5 . .
O6 C8 H8B 109.5 . .
C7 C8 H8A 109.5 . .
C7 C8 H8B 109.5 . .
H8A C8 H8B 108.1 . .
O5 C9 H9A 109.6 . .
O5 C9 H9B 109.6 . .
O5 C9 C10 110.31(19) . .
H9A C9 H9B 108.1 . .
C10 C9 H9A 109.6 . .
C10 C9 H9B 109.6 . .
O6 C10 C9 110.22(18) . .
O6 C10 H10A 109.6 . .
O6 C10 H10B 109.6 . .
C9 C10 H10A 109.6 . .
C9 C10 H10B 109.6 . .
H10A C10 H10B 108.1 . .
O7 C11 H11A 109.7 . .
O7 C11 H11B 109.7 . .
O7 C11 C12 109.89(19) . .
H11A C11 H11B 108.2 . .
C12 C11 H11A 109.7 . .
C12 C11 H11B 109.7 . .
O8 C12 C11 110.82(18) . .
O8 C12 H12A 109.5 . .
O8 C12 H12B 109.5 . .
C11 C12 H12A 109.5 . .
C11 C12 H12B 109.5 . .
H12A C12 H12B 108.1 . .
O7 C13 H13A 109.4 . .
O7 C13 H13B 109.4 . .
O7 C13 C14 111.04(18) . .
H13A C13 H13B 108.0 . .
C14 C13 H13A 109.4 . .
C14 C13 H13B 109.4 . .
O8 C14 C13 110.04(18) . .
O8 C14 H14A 109.7 . .
O8 C14 H14B 109.7 . .
C13 C14 H14A 109.7 . .
C13 C14 H14B 109.7 . .
H14A C14 H14B 108.2 . .
O9 C15 H15A 109.5 . .
O9 C15 H15B 109.5 . .
O9 C15 C16 110.88(19) . .
H15A C15 H15B 108.1 . .
C16 C15 H15A 109.5 . .
C16 C15 H15B 109.5 . .
O10 C16 C15 110.74(18) . .
O10 C16 H16A 109.5 . .
O10 C16 H16B 109.5 . .
C15 C16 H16A 109.5 . .
C15 C16 H16B 109.5 . .
H16A C16 H16B 108.1 . .
O9 C17 H17A 109.6 . .
O9 C17 H17B 109.6 . .
O9 C17 C18 110.39(18) . .
H17A C17 H17B 108.1 . .
C18 C17 H17A 109.6 . .
C18 C17 H17B 109.6 . .
O10 C18 C17 110.45(18) . .
O10 C18 H18A 109.6 . .
O10 C18 H18B 109.6 . .
C17 C18 H18A 109.6 . .
C17 C18 H18B 109.6 . .
H18A C18 H18B 108.1 . .
O11 C19 H19A 109.5 . .
O11 C19 H19B 109.5 . .
O11 C19 C20 110.81(18) . .
H19A C19 H19B 108.1 . .
C20 C19 H19A 109.5 . .
C20 C19 H19B 109.5 . .
O12 C20 C19 110.4(2) . .
O12 C20 H20A 109.6 . .
O12 C20 H20B 109.6 . .
C19 C20 H20A 109.6 . .
C19 C20 H20B 109.6 . .
H20A C20 H20B 108.1 . .
O11 C21 H21A 109.6 . .
O11 C21 H21B 109.6 . .
O11 C21 C22 110.38(19) . .
H21A C21 H21B 108.1 . .
C22 C21 H21A 109.6 . .
C22 C21 H21B 109.6 . .
O12 C22 C21 110.31(18) . .
O12 C22 H22A 109.6 . .
O12 C22 H22B 109.6 . .
C21 C22 H22A 109.6 . .
C21 C22 H22B 109.6 . .
H22A C22 H22B 108.1 . .
O13 C23 H23A 109.5 . .
O13 C23 H23B 109.5 . .
O13 C23 C24 110.80(18) . .
H23A C23 H23B 108.1 . .
C24 C23 H23A 109.5 . .
C24 C23 H23B 109.5 . .
O14 C24 C23 110.37(17) . .
O14 C24 H24A 109.6 . .
O14 C24 H24B 109.6 . .
C23 C24 H24A 109.6 . .
C23 C24 H24B 109.6 . .
H24A C24 H24B 108.1 . .
O13 C25 H25A 109.6 . .
O13 C25 H25B 109.6 . .
O13 C25 C26 110.24(18) . .
H25A C25 H25B 108.1 . .
C26 C25 H25A 109.6 . .
C26 C25 H25B 109.6 . .
O14 C26 C25 110.38(18) . .
O14 C26 H26A 109.6 . .
O14 C26 H26B 109.6 . .
C25 C26 H26A 109.6 . .
C25 C26 H26B 109.6 . .
H26A C26 H26B 108.1 . .
O1 C1 P1 178.6(3) . .
O2A C2A P2A 175.1(7) . .
O2B C2B P2B 164(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Na1 O3 2.3811(19) .
Na1 O4 2.3639(18) 2_564
Na1 O5 2.3902(17) .
Na1 O7 2.3587(17) .
Na1 O10 2.4051(17) 1_545
Na1 O14 2.3506(17) 1_645
Na2 O6 2.4061(17) 1_455
Na2 O8 2.3411(17) .
Na2 O9 2.4274(17) .
Na2 O11 2.3603(19) .
Na2 O12 2.3780(18) 2_575
Na2 O13 2.3507(17) .
O3 C3 1.443(3) .
O3 C5 1.437(3) .
O4 Na1 2.3639(18) 2_565
O4 C4 1.434(3) .
O4 C6 1.434(3) .
O5 C7 1.436(3) .
O5 C9 1.436(3) .
O6 Na2 2.4061(17) 1_655
O6 C8 1.439(3) .
O6 C10 1.438(3) .
O7 C11 1.440(3) .
O7 C13 1.431(3) .
O8 C12 1.432(3) .
O8 C14 1.431(3) .
O9 C15 1.436(3) .
O9 C17 1.440(3) .
O10 Na1 2.4051(17) 1_565
O10 C16 1.439(3) .
O10 C18 1.439(3) .
O11 C19 1.434(3) .
O11 C21 1.432(3) .
O12 Na2 2.3781(18) 2_574
O12 C20 1.436(3) .
O12 C22 1.435(3) .
O13 C23 1.437(3) .
O13 C25 1.436(3) .
O14 Na1 2.3506(16) 1_465
O14 C24 1.437(3) .
O14 C26 1.435(3) .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C3 C4 1.504(3) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C5 C6 1.516(3) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C7 C8 1.514(3) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C9 C10 1.514(3) .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C11 C12 1.513(3) .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
C13 H13A 0.9700 .
C13 H13B 0.9700 .
C13 C14 1.513(3) .
C14 H14A 0.9700 .
C14 H14B 0.9700 .
C15 H15A 0.9700 .
C15 H15B 0.9700 .
C15 C16 1.513(3) .
C16 H16A 0.9700 .
C16 H16B 0.9700 .
C17 H17A 0.9700 .
C17 H17B 0.9700 .
C17 C18 1.514(3) .
C18 H18A 0.9700 .
C18 H18B 0.9700 .
C19 H19A 0.9700 .
C19 H19B 0.9700 .
C19 C20 1.513(3) .
C20 H20A 0.9700 .
C20 H20B 0.9700 .
C21 H21A 0.9700 .
C21 H21B 0.9700 .
C21 C22 1.514(3) .
C22 H22A 0.9700 .
C22 H22B 0.9700 .
C23 H23A 0.9700 .
C23 H23B 0.9700 .
C23 C24 1.515(3) .
C24 H24A 0.9700 .
C24 H24B 0.9700 .
C25 H25A 0.9700 .
C25 H25B 0.9700 .
C25 C26 1.512(3) .
C26 H26A 0.9700 .
C26 H26B 0.9700 .
P1 C1 1.634(3) .
O1 C1 1.163(4) .
P2A C2A 1.655(6) .
O2A C2A 1.133(7) .
P2B C2B 1.62(2) .
O2B C2B 1.14(2) .
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
Na1 O3 C3 C4 -126.74(17) .
Na1 O3 C5 C6 127.27(17) .
Na1 O4 C4 C3 -129.18(16) 2_565
Na1 O4 C6 C5 130.10(16) 2_565
Na1 O5 C7 C8 -122.38(17) .
Na1 O5 C9 C10 121.76(16) .
Na1 O7 C11 C12 -148.76(16) .
Na1 O7 C13 C14 144.70(15) .
Na1 O10 C16 C15 131.09(16) 1_565
Na1 O10 C18 C17 -130.51(15) 1_565
Na1 O14 C24 C23 -145.87(15) 1_465
Na1 O14 C26 C25 145.69(15) 1_465
Na2 O6 C8 C7 -121.04(18) 1_655
Na2 O6 C10 C9 120.70(16) 1_655
Na2 O8 C12 C11 -143.67(15) .
Na2 O8 C14 C13 145.54(16) .
Na2 O9 C15 C16 126.90(16) .
Na2 O9 C17 C18 -126.34(17) .
Na2 O11 C19 C20 -128.53(16) .
Na2 O11 C21 C22 128.46(16) .
Na2 O12 C20 C19 -129.87(16) 2_574
Na2 O12 C22 C21 129.66(16) 2_574
Na2 O13 C23 C24 -142.33(15) .
Na2 O13 C25 C26 140.87(15) .
O3 C3 C4 O4 -59.5(2) .
O3 C5 C6 O4 59.2(2) .
O5 C7 C8 O6 -58.3(2) .
O5 C9 C10 O6 59.5(2) .
O7 C11 C12 O8 -58.3(2) .
O7 C13 C14 O8 58.2(2) .
O9 C15 C16 O10 58.5(2) .
O9 C17 C18 O10 -59.8(2) .
O11 C19 C20 O12 -58.7(2) .
O11 C21 C22 O12 59.6(2) .
O13 C23 C24 O14 -57.8(2) .
O13 C25 C26 O14 59.3(2) .
C3 O3 C5 C6 -58.4(2) .
C4 O4 C6 C5 -58.2(2) .
C5 O3 C3 C4 58.6(2) .
C6 O4 C4 C3 58.6(2) .
C7 O5 C9 C10 -59.0(2) .
C8 O6 C10 C9 -58.1(2) .
C9 O5 C7 C8 58.4(2) .
C10 O6 C8 C7 57.6(2) .
C11 O7 C13 C14 -58.0(2) .
C12 O8 C14 C13 -57.7(2) .
C13 O7 C11 C12 57.6(2) .
C14 O8 C12 C11 58.4(2) .
C15 O9 C17 C18 57.8(2) .
C16 O10 C18 C17 59.1(2) .
C17 O9 C15 C16 -57.3(2) .
C18 O10 C16 C15 -58.5(2) .
C19 O11 C21 C22 -58.1(2) .
C20 O12 C22 C21 -59.1(2) .
C21 O11 C19 C20 57.8(2) .
C22 O12 C20 C19 58.5(2) .
C23 O13 C25 C26 -58.2(2) .
C24 O14 C26 C25 -58.7(2) .
C25 O13 C23 C24 57.7(2) .
C26 O14 C24 C23 57.8(2) .
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0000 0.0003 -0.9996 -0.0150 0.1007 -0.0189
-4.9952 -3.9991 1.9967 -0.8957 -0.2673 -0.0283
-0.0000 -0.0003 0.9996 0.0150 -0.1007 0.0189
3.9992 -4.9954 -2.0001 0.0307 -0.0263 -0.9430
-3.9992 4.9954 2.0001 -0.0307 0.0263 0.9430
3.9992 -4.9971 3.9978 0.1208 -0.6306 -0.8296
4.9959 2.0007 -2.9971 0.7148 0.2996 -0.2243
-0.0011 2.9995 -4.9972 0.1737 0.6062 0.2560
-3.9992 4.9945 4.9990 0.0143 -0.2758 0.9997
-1.9971 -3.9964 -5.0001 -0.6443 0.3952 -0.4013
1.0001 -1.9971 -4.9987 -0.1221 0.4210 -0.4084
4.9959 1.9983 5.0001 0.8349 -0.5061 -0.0731
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.54(2)
2 0.46(2)
