#------------------------------------------------------------------------------
#$Date: 2017-08-02 05:43:30 +0300 (Wed, 02 Aug 2017) $
#$Revision: 199449 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/38/7043870.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_7043870
loop_
_publ_author_name
'Behm, Kira'
'Essner, Jeremy B.'
'Barnes, Charles L.'
'Baker, Gary A.'
'Walensky, Justin R.'
_publ_section_title
;
 Synthesis and fluorescence spectroscopy of tris(pyrenyl)pnictogen
 compounds
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01953J
_journal_year                    2017
_chemical_formula_moiety         'C48 H27 O1 P, 0.5(H2 O)'
_chemical_formula_sum            'C48 H27 O1.5 P'
_chemical_formula_weight         658.66
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-07-07 deposited with the CCDC.
2017-07-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   19.6411(11)
_cell_length_b                   19.6411(11)
_cell_length_c                   19.5128(10)
_cell_measurement_reflns_used    3142
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.3
_cell_measurement_theta_min      2.6
_cell_volume                     6519.0(6)
_computing_cell_refinement       'SAINT. Ver. 8.34A. (Bruker-AXS, 2014)'
_computing_data_collection       'APEX3. Ver. 2017.3-0.  (Bruker-AXS, 2017)'
_computing_data_reduction        'SAINT. Ver. 8.34A. (Bruker-AXS, 2014)'
_computing_molecular_graphics    'X-Seed (Barbour, 2001)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'XL. Ver. 2014/7. (Sheldrick, 2015b)'
_computing_structure_solution    'XT. Ver. 2014/4. (Sheldrick, 2015a)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker VENTURE CMOS area detector'
_diffrn_measurement_method       'shutterless omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7469
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.374
_diffrn_reflns_theta_min         2.612
_diffrn_source                   'Incoatec IMuS microfocus Mo tube'
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Data were corrected for decay and absorption using the program SADABS 
 (Sheldrick, G. M. (2003). SADABS. Version 2.10. University of
 Göttingen, Germany).
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.007
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2052
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.395
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         2972
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.0622
_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)+(0.0942P)²+7.9727P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1701
_refine_ls_wR_factor_ref         0.1865
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2075
_reflns_number_total             2972
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt01953j2.cif
_cod_data_source_block           KBN-1-22
_cod_original_cell_volume        6519.0(8)
_cod_original_formula_sum        'C48 H27 O1.50 P'
_cod_database_code               7043870
_shelx_shelxl_version_number     2014/7
_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.
;
_shelx_estimated_absorpt_t_min   0.977
_shelx_estimated_absorpt_t_max   0.986
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
P1 P 0.3333 0.6667 0.47124(5) 0.0311(3) Uani 1 3 d S T P . .
O1 O 0.3333 0.6667 0.54714(17) 0.0603(9) Uani 1 3 d S T P . .
C1 C 0.39063(12) 0.62651(13) 0.43300(12) 0.0316(5) Uani 1 1 d . . . . .
C2 C 0.44043(14) 0.66578(14) 0.37820(12) 0.0399(6) Uani 1 1 d . . . . .
H2 H 0.4454 0.7140 0.3629 0.048 Uiso 1 1 calc R U . . .
C3 C 0.48272(15) 0.63667(15) 0.34557(13) 0.0448(6) Uani 1 1 d . . . . .
H3 H 0.5158 0.6647 0.3081 0.054 Uiso 1 1 calc R U . . .
C4 C 0.47754(14) 0.56663(14) 0.36689(12) 0.0380(6) Uani 1 1 d . . . . .
C5 C 0.42823(12) 0.52569(13) 0.42302(12) 0.0322(5) Uani 1 1 d . . . . .
C6 C 0.38363(12) 0.55534(13) 0.45628(11) 0.0315(5) Uani 1 1 d . . . . .
C7 C 0.33358(13) 0.51010(13) 0.51221(13) 0.0370(6) Uani 1 1 d . . . . .
H7 H 0.3026 0.5280 0.5347 0.044 Uiso 1 1 calc R U . . .
C8 C 0.32964(14) 0.44270(14) 0.53346(14) 0.0424(6) Uani 1 1 d . . . . .
H8 H 0.2966 0.4150 0.5710 0.051 Uiso 1 1 calc R U . . .
C9 C 0.37392(14) 0.41194(13) 0.50092(13) 0.0401(6) Uani 1 1 d . . . . .
C10 C 0.42298(13) 0.45363(13) 0.44542(13) 0.0360(6) Uani 1 1 d . . . . .
C11 C 0.46801(14) 0.42507(15) 0.41205(13) 0.0419(6) Uani 1 1 d . . . . .
C12 C 0.46279(16) 0.35564(16) 0.43578(15) 0.0513(8) Uani 1 1 d . . . . .
H12 H 0.4929 0.3362 0.4140 0.062 Uiso 1 1 calc R U . . .
C13 C 0.41513(17) 0.31490(15) 0.48975(17) 0.0546(8) Uani 1 1 d . . . . .
H13 H 0.4124 0.2675 0.5046 0.066 Uiso 1 1 calc R U . . .
C14 C 0.37104(16) 0.34204(15) 0.52275(15) 0.0510(7) Uani 1 1 d . . . . .
H14 H 0.3386 0.3135 0.5604 0.061 Uiso 1 1 calc R U . . .
C15 C 0.51747(16) 0.46908(17) 0.35593(14) 0.0507(7) Uani 1 1 d . . . . .
H15 H 0.5479 0.4504 0.3336 0.061 Uiso 1 1 calc R U . . .
C16 C 0.52188(15) 0.53407(17) 0.33467(13) 0.0474(7) Uani 1 1 d . . . . .
H16 H 0.5551 0.5611 0.2969 0.057 Uiso 1 1 calc R U . . .
O1S O 0.2460(7) 0.5882(9) 0.6655(5) 0.075(4) Uani 0.1666 1 d . . P A -1
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'
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_
_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
O1 P1 C1 114.13(8) . 2_665
O1 P1 C1 114.13(8) . 3_565
C1 P1 C1 104.44(9) 2_665 3_565
O1 P1 C1 114.13(8) . .
C1 P1 C1 104.44(9) 2_665 .
C1 P1 C1 104.44(9) 3_565 .
C2 C1 C6 119.3(2) . .
C2 C1 P1 119.24(17) . .
C6 C1 P1 121.41(17) . .
C3 C2 C1 121.8(2) . .
C3 C2 H2 119.1 . .
C1 C2 H2 119.1 . .
C2 C3 C4 120.7(2) . .
C2 C3 H3 119.6 . .
C4 C3 H3 119.6 . .
C3 C4 C5 118.9(2) . .
C3 C4 C16 122.8(2) . .
C5 C4 C16 118.3(2) . .
C4 C5 C6 120.3(2) . .
C4 C5 C10 119.2(2) . .
C6 C5 C10 120.5(2) . .
C1 C6 C5 118.9(2) . .
C1 C6 C7 123.7(2) . .
C5 C6 C7 117.5(2) . .
C8 C7 C6 121.6(2) . .
C8 C7 H7 119.2 . .
C6 C7 H7 119.2 . .
C7 C8 C9 121.9(2) . .
C7 C8 H8 119.1 . .
C9 C8 H8 119.1 . .
C10 C9 C14 118.7(2) . .
C10 C9 C8 118.6(2) . .
C14 C9 C8 122.6(2) . .
C9 C10 C11 120.2(2) . .
C9 C10 C5 119.9(2) . .
C11 C10 C5 119.9(2) . .
C12 C11 C10 118.6(3) . .
C12 C11 C15 122.7(2) . .
C10 C11 C15 118.7(2) . .
C13 C12 C11 121.4(3) . .
C13 C12 H12 119.3 . .
C11 C12 H12 119.3 . .
C12 C13 C14 120.6(3) . .
C12 C13 H13 119.7 . .
C14 C13 H13 119.7 . .
C13 C14 C9 120.4(3) . .
C13 C14 H14 119.8 . .
C9 C14 H14 119.8 . .
C16 C15 C11 121.8(2) . .
C16 C15 H15 119.1 . .
C11 C15 H15 119.1 . .
C15 C16 C4 122.1(3) . .
C15 C16 H16 119.0 . .
C4 C16 H16 119.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
P1 O1 1.481(3) .
P1 C1 1.826(2) 2_665
P1 C1 1.826(2) 3_565
P1 C1 1.826(2) .
C1 C2 1.393(3) .
C1 C6 1.410(3) .
C2 C3 1.377(3) .
C2 H2 0.9500 .
C3 C4 1.391(3) .
C3 H3 0.9500 .
C4 C5 1.416(3) .
C4 C16 1.456(3) .
C5 C6 1.428(3) .
C5 C10 1.435(3) .
C6 C7 1.440(3) .
C7 C8 1.352(3) .
C7 H7 0.9500 .
C8 C9 1.432(4) .
C8 H8 0.9500 .
C9 C10 1.408(4) .
C9 C14 1.411(3) .
C10 C11 1.420(3) .
C11 C12 1.395(4) .
C11 C15 1.432(4) .
C12 C13 1.370(4) .
C12 H12 0.9500 .
C13 C14 1.382(4) .
C13 H13 0.9500 .
C14 H14 0.9500 .
C15 C16 1.303(4) .
C15 H15 0.9500 .
C16 H16 0.9500 .
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
O1 P1 C1 C2 -135.49(17) .
C1 P1 C1 C2 -10.2(2) 2_665
C1 P1 C1 C2 99.21(14) 3_565
O1 P1 C1 C6 46.6(2) .
C1 P1 C1 C6 171.89(17) 2_665
C1 P1 C1 C6 -78.7(3) 3_565
C6 C1 C2 C3 0.6(4) .
P1 C1 C2 C3 -177.40(19) .
C1 C2 C3 C4 -0.6(4) .
C2 C3 C4 C5 -0.3(4) .
C2 C3 C4 C16 -179.1(2) .
C3 C4 C5 C6 1.1(3) .
C16 C4 C5 C6 180.0(2) .
C3 C4 C5 C10 -179.7(2) .
C16 C4 C5 C10 -0.8(3) .
C2 C1 C6 C5 0.3(3) .
P1 C1 C6 C5 178.17(16) .
C2 C1 C6 C7 -179.7(2) .
P1 C1 C6 C7 -1.8(3) .
C4 C5 C6 C1 -1.1(3) .
C10 C5 C6 C1 179.7(2) .
C4 C5 C6 C7 178.9(2) .
C10 C5 C6 C7 -0.3(3) .
C1 C6 C7 C8 -179.0(2) .
C5 C6 C7 C8 1.1(3) .
C6 C7 C8 C9 -1.0(4) .
C7 C8 C9 C10 0.2(4) .
C7 C8 C9 C14 179.5(2) .
C14 C9 C10 C11 0.5(3) .
C8 C9 C10 C11 179.8(2) .
C14 C9 C10 C5 -178.8(2) .
C8 C9 C10 C5 0.5(3) .
C4 C5 C10 C9 -179.7(2) .
C6 C5 C10 C9 -0.4(3) .
C4 C5 C10 C11 1.1(3) .
C6 C5 C10 C11 -179.7(2) .
C9 C10 C11 C12 -0.4(3) .
C5 C10 C11 C12 178.8(2) .
C9 C10 C11 C15 -179.8(2) .
C5 C10 C11 C15 -0.5(3) .
C10 C11 C12 C13 0.4(4) .
C15 C11 C12 C13 179.8(2) .
C11 C12 C13 C14 -0.5(4) .
C12 C13 C14 C9 0.5(4) .
C10 C9 C14 C13 -0.5(4) .
C8 C9 C14 C13 -179.8(2) .
C12 C11 C15 C16 -179.7(2) .
C10 C11 C15 C16 -0.3(4) .
C11 C15 C16 C4 0.6(4) .
C3 C4 C16 C15 178.8(3) .
C5 C4 C16 C15 -0.1(4) .
