#------------------------------------------------------------------------------
#$Date: 2017-10-04 18:03:55 +0300 (Wed, 04 Oct 2017) $
#$Revision: 201609 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/65/4126518.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_4126518
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_formula_moiety         'C O P, Na'
_chemical_formula_sum            'C Na O P'
_chemical_formula_weight         81.97
_space_group_crystal_system      hexagonal
_space_group_IT_number           190
_space_group_name_Hall           'P -6c -2c'
_space_group_name_H-M_alt        'P -6 2 c'
_symmetry_space_group_name_Hall  'P -6c -2c'
_symmetry_space_group_name_H-M   'P -6 2 c'
_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                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   8.5229(19)
_cell_length_b                   8.5229(19)
_cell_length_c                   7.178(2)
_cell_measurement_reflns_used    496
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.0610
_cell_measurement_theta_min      4.7650
_cell_volume                     451.55(19)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2850
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω      6.00  83.10   0.30   20.00    --    9.82  77.00 120.00  257
  2  ω    -20.00  49.00   0.30   20.00    --    9.82 -99.00 150.00  230
  3  ω    -16.00  26.00   0.30   20.00    --   -9.97 -99.00 120.00  140
  4  ω    -53.00 -11.00   0.30   20.00    --   -9.97 -38.00   0.00  140
;
_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      0.0391837000
_diffrn_orient_matrix_UB_12      0.0115958000
_diffrn_orient_matrix_UB_13      -0.0897287000
_diffrn_orient_matrix_UB_21      0.0144529000
_diffrn_orient_matrix_UB_22      0.0895550000
_diffrn_orient_matrix_UB_23      -0.0037593000
_diffrn_orient_matrix_UB_31      0.0866111000
_diffrn_orient_matrix_UB_32      0.0332025000
_diffrn_orient_matrix_UB_33      0.0411211000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2556
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.695
_diffrn_reflns_theta_min         2.760
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.757
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.903
_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    1.809
_exptl_crystal_description       needle
_exptl_crystal_F_000             240
_exptl_crystal_size_max          0.278
_exptl_crystal_size_mid          0.038
_exptl_crystal_size_min          0.028
_refine_diff_density_max         1.419
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.216
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.185
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     25
_refine_ls_number_reflns         348
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0755
_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)+(0.1205P)²+1.6505P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2004
_refine_ls_wR_factor_ref         0.2103
_reflns_Friedel_coverage         0.662
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                300
_reflns_number_total             348
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja7b07704_si_031.cif
_cod_data_source_block           NaOCP_1
_cod_original_cell_volume        451.6(2)
_cod_database_code               4126518
_chemical_oxdiff_formula         'Na O C P'
_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 99.57
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.67
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1.3(13) -0.3(13)
;
_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 1.485
_oxdiff_exptl_absorpt_empirical_full_min 0.683
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x, y, -z+1/2'
'-y, x-y, -z+1/2'
'-x+y, -x, -z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, z+1/2'
'x-y, -y, z+1/2'
'-x, -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
P1 P 1.1975(5) 0.3366(5) 0.7500 0.0179(10) Uani 1 2 d S T P
Na1 Na 1.0000 0.0000 0.5000 0.0150(19) Uani 1 6 d S T P
Na2 Na 0.6667 0.3333 0.5160(8) 0.0137(15) Uani 1 3 d S T P
O1 O 0.8738(15) 0.3423(12) 0.7500 0.025(3) Uani 1 2 d S T P
C1 C 1.008(2) 0.3382(16) 0.7500 0.015(3) Uani 1 2 d S T P
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'
Na Na 0.0362 0.0249 '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'
P P 0.1023 0.0942 '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
1 0 0 0.0169
1 -1 0 0.0141
-1 1 0 0.0141
0 -1 0 0.0162
0 1 0 0.0162
0 0 -1 0.1392
0 0 1 0.1392
-1 0 0 0.0169
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
Na1 P1 Na1 71.40(8) . 4_556
Na1 P1 Na2 170.50(12) . 10_655
Na1 P1 Na2 170.50(12) 4_556 7_656
Na1 P1 Na2 105.58(9) . 7_656
Na1 P1 Na2 105.58(9) 4_556 10_655
Na2 P1 Na2 75.9(2) 10_655 7_656
C1 P1 Na1 85.7(3) . 4_556
C1 P1 Na1 85.7(3) . .
C1 P1 Na2 85.1(3) . 7_656
C1 P1 Na2 85.1(3) . 10_655
P1 Na1 P1 170.73(13) 7_646 2_645
P1 Na1 P1 97.50(11) 9_766 .
P1 Na1 P1 170.73(13) 8_556 .
P1 Na1 P1 89.38(6) 2_645 3_765
P1 Na1 P1 97.50(11) 8_556 2_645
P1 Na1 P1 97.50(11) 7_646 3_765
P1 Na1 P1 84.51(10) 7_646 .
P1 Na1 P1 89.38(6) 8_556 7_646
P1 Na1 P1 89.38(6) 3_765 .
P1 Na1 P1 84.51(10) 8_556 3_765
P1 Na1 P1 170.73(13) 9_766 3_765
P1 Na1 P1 89.38(6) 8_556 9_766
P1 Na1 P1 89.38(6) 2_645 .
P1 Na1 P1 89.38(6) 9_766 7_646
P1 Na1 P1 84.51(10) 9_766 2_645
P1 Na1 Na1 125.70(4) 8_556 4_556
P1 Na1 Na1 54.30(4) . 4_556
P1 Na1 Na1 54.30(4) 2_645 4_556
P1 Na1 Na1 125.70(4) 3_765 4
P1 Na1 Na1 54.30(4) 3_765 4_556
P1 Na1 Na1 54.30(4) 9_766 4
P1 Na1 Na1 125.70(4) 9_766 4_556
P1 Na1 Na1 54.30(4) 7_646 4
P1 Na1 Na1 125.70(4) 7_646 4_556
P1 Na1 Na1 125.70(4) 2_645 4
P1 Na1 Na1 54.30(4) 8_556 4
P1 Na1 Na1 125.70(4) . 4
Na1 Na1 Na1 180.0 4_556 4
P1 Na2 P1 86.15(14) 9_766 7_546
P1 Na2 P1 86.15(14) 9_766 8_566
P1 Na2 P1 86.15(14) 8_566 7_546
P1 Na2 Na2 127.94(10) 9_766 4_556
P1 Na2 Na2 127.94(10) 8_566 4_556
P1 Na2 Na2 52.06(10) 8_566 4
P1 Na2 Na2 52.06(10) 9_766 4
P1 Na2 Na2 52.06(10) 7_546 4
P1 Na2 Na2 127.94(10) 7_546 4_556
Na2 Na2 Na2 180.0 4_556 4
O1 Na2 P1 89.02(19) . 9_766
O1 Na2 P1 162.4(2) . 7_546
O1 Na2 P1 162.4(2) 3_665 8_566
O1 Na2 P1 89.02(19) 2_655 8_566
O1 Na2 P1 162.4(2) 2_655 9_766
O1 Na2 P1 89.02(19) 3_665 7_546
O1 Na2 P1 110.5(2) 2_655 7_546
O1 Na2 P1 110.5(2) 3_665 9_766
O1 Na2 P1 110.5(2) . 8_566
O1 Na2 Na2 134.2(2) 2_655 4
O1 Na2 Na2 45.8(2) 3_665 4_556
O1 Na2 Na2 134.2(2) 3_665 4
O1 Na2 Na2 45.8(2) . 4_556
O1 Na2 Na2 45.8(2) 2_655 4_556
O1 Na2 Na2 134.2(2) . 4
O1 Na2 O1 76.8(3) . 3_665
O1 Na2 O1 76.8(3) . 2_655
O1 Na2 O1 76.8(3) 3_665 2_655
Na2 O1 Na2 88.4(4) 4_556 .
C1 O1 Na2 135.7(2) . .
C1 O1 Na2 135.7(2) . 4_556
O1 C1 P1 178.9(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
P1 Na1 3.075(3) .
P1 Na1 3.075(3) 4_556
P1 Na2 3.105(5) 10_655
P1 Na2 3.105(5) 7_656
P1 C1 1.622(15) .
Na1 P1 3.075(3) 7_646
Na1 P1 3.075(3) 9_766
Na1 P1 3.075(3) 3_765
Na1 P1 3.075(3) 8_556
Na1 P1 3.075(3) 2_645
Na1 Na1 3.5891(10) 4
Na1 Na1 3.5891(10) 4_556
Na2 P1 3.105(5) 9_766
Na2 P1 3.105(5) 7_546
Na2 P1 3.105(5) 8_566
Na2 Na2 3.818(12) 4
Na2 Na2 3.360(12) 4_556
Na2 O1 2.411(9) 3_665
Na2 O1 2.411(9) 2_655
Na2 O1 2.411(9) .
O1 Na2 2.411(9) 4_556
O1 C1 1.16(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
0.9992 0.0001 -0.0001 0.0392 0.0145 0.0865
0.9992 -0.9991 0.0004 0.0275 -0.0750 0.0534
-0.9992 0.9991 -0.0004 -0.0275 0.0750 -0.0534
-0.0000 -0.9992 0.0005 -0.0116 -0.0895 -0.0332
0.0000 0.9992 -0.0005 0.0116 0.0895 0.0332
0.0002 -0.0010 -1.0001 0.0897 0.0037 -0.0411
-0.0002 0.0010 1.0001 -0.0897 -0.0037 0.0411
-0.9992 -0.0001 0.0001 -0.0392 -0.0145 -0.0865
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 1.3(13)
2 -0.3(13)
