#------------------------------------------------------------------------------
#$Date: 2019-11-03 13:50:43 +0200 (Sun, 03 Nov 2019) $
#$Revision: 221578 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/84/4128476.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_4128476
loop_
_publ_author_name
'Arz, Marius I.'
'Annibale, Vincent T.'
'Kelly, Nicole L.'
'Hanna, John V.'
'Manners, Ian'
_publ_section_title
;
 Ring-Opening Polymerization of Cyclic Phosphonates: Access to Inorganic
 Polymers with a PV-O Main Chain.
;
_journal_issue                   7
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2894
_journal_page_last               2899
_journal_paper_doi               10.1021/jacs.8b13435
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C36 H30 O12 P6'
_chemical_formula_sum            'C36 H30 O12 P6'
_chemical_formula_weight         840.42
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-11-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                114.987(2)
_cell_angle_beta                 104.507(2)
_cell_angle_gamma                94.529(2)
_cell_formula_units_Z            1
_cell_length_a                   8.7802(3)
_cell_length_b                   11.2721(4)
_cell_length_c                   12.4055(5)
_cell_measurement_reflns_used    3160
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.31
_cell_measurement_theta_min      2.45
_cell_volume                     1053.23(7)
_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_temperature      100.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_unetI/netI     0.0501
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14318
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.548
_diffrn_reflns_theta_min         1.908
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.312
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0696 before and 0.0432 after correction. The Ratio of minimum to maximum transmission is 0.7614. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       prism
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.498
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.065
_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     244
_refine_ls_number_reflns         4831
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0527P)²+0.0575P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0967
_refine_ls_wR_factor_ref         0.1038
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3633
_reflns_number_total             4831
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja8b13435_si_002.cif
_cod_data_source_block           1Ph6
_cod_database_code               4128476
_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_max   0.955
_shelx_estimated_absorpt_t_min   0.896
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
P1 P 0.38918(6) 0.24759(5) 0.33919(5) 0.01451(13) Uani 1 1 d .
P2 P 0.50878(6) 0.29130(5) 0.59590(5) 0.01379(13) Uani 1 1 d .
P3 P 0.46530(6) 0.56547(5) 0.72905(5) 0.01452(13) Uani 1 1 d .
O1 O 0.47697(18) 0.14608(14) 0.28390(14) 0.0213(3) Uani 1 1 d .
O2 O 0.39369(16) 0.36561(14) 0.30010(13) 0.0157(3) Uani 1 1 d .
O3 O 0.46496(17) 0.33710(13) 0.48796(13) 0.0154(3) Uani 1 1 d .
O4 O 0.38777(17) 0.18384(14) 0.57863(14) 0.0188(3) Uani 1 1 d .
O5 O 0.52580(17) 0.43156(13) 0.71417(13) 0.0161(3) Uani 1 1 d .
O6 O 0.30520(17) 0.54756(14) 0.64726(13) 0.0198(3) Uani 1 1 d .
C1 C 0.1817(3) 0.1929(2) 0.3058(2) 0.0171(4) Uani 1 1 d .
C2 C 0.1065(3) 0.0635(2) 0.2126(2) 0.0302(6) Uani 1 1 d .
H2 H 0.1673 0.0054 0.1694 0.036 Uiso 1 1 calc R
C3 C -0.0575(3) 0.0199(3) 0.1834(3) 0.0386(7) Uani 1 1 d .
H3 H -0.1093 -0.0680 0.1194 0.046 Uiso 1 1 calc R
C4 C -0.1457(3) 0.1036(2) 0.2466(2) 0.0317(6) Uani 1 1 d .
H4 H -0.2578 0.0727 0.2270 0.038 Uiso 1 1 calc R
C5 C -0.0715(3) 0.2321(2) 0.3384(2) 0.0272(5) Uani 1 1 d .
H5 H -0.1335 0.2899 0.3803 0.033 Uiso 1 1 calc R
C6 C 0.0913(3) 0.2774(2) 0.3697(2) 0.0233(5) Uani 1 1 d .
H6 H 0.1420 0.3653 0.4342 0.028 Uiso 1 1 calc R
C7 C 0.7072(2) 0.2650(2) 0.61398(19) 0.0161(4) Uani 1 1 d .
C8 C 0.7330(3) 0.1371(2) 0.5894(2) 0.0223(5) Uani 1 1 d .
H8 H 0.6461 0.0673 0.5687 0.027 Uiso 1 1 calc R
C9 C 0.8865(3) 0.1121(2) 0.5955(2) 0.0279(5) Uani 1 1 d .
H9 H 0.9051 0.0252 0.5792 0.033 Uiso 1 1 calc R
C10 C 1.0112(3) 0.2132(3) 0.6251(2) 0.0290(6) Uani 1 1 d .
H10 H 1.1157 0.1952 0.6281 0.035 Uiso 1 1 calc R
C11 C 0.9874(3) 0.3410(3) 0.6506(2) 0.0302(6) Uani 1 1 d .
H11 H 1.0752 0.4103 0.6718 0.036 Uiso 1 1 calc R
C12 C 0.8347(3) 0.3675(2) 0.6451(2) 0.0243(5) Uani 1 1 d .
H12 H 0.8173 0.4549 0.6624 0.029 Uiso 1 1 calc R
C13 C 0.5011(3) 0.6570(2) 0.8920(2) 0.0191(5) Uani 1 1 d .
C14 C 0.4348(3) 0.7700(3) 0.9328(2) 0.0341(6) Uani 1 1 d .
H14 H 0.3697 0.7927 0.8736 0.041 Uiso 1 1 calc R
C15 C 0.4636(3) 0.8493(3) 1.0598(2) 0.0382(7) Uani 1 1 d .
H15 H 0.4212 0.9280 1.0878 0.046 Uiso 1 1 calc R
C16 C 0.5535(3) 0.8141(2) 1.1451(2) 0.0341(6) Uani 1 1 d .
H16 H 0.5703 0.8670 1.2320 0.041 Uiso 1 1 calc R
C17 C 0.6188(3) 0.7039(3) 1.1056(2) 0.0371(6) Uani 1 1 d .
H17 H 0.6813 0.6806 1.1653 0.044 Uiso 1 1 calc R
C18 C 0.5949(3) 0.6247(2) 0.9786(2) 0.0293(6) Uani 1 1 d .
H18 H 0.6428 0.5491 0.9519 0.035 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'
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 O2 115.08(8) . .
O1 P1 O3 114.47(8) . .
O1 P1 C1 116.79(10) . .
O2 P1 O3 98.24(7) . .
O2 P1 C1 102.50(8) . .
O3 P1 C1 107.57(9) . .
O3 P2 O5 98.93(7) . .
O3 P2 C7 106.75(9) . .
O4 P2 O3 113.83(8) . .
O4 P2 O5 114.08(8) . .
O4 P2 C7 116.85(9) . .
O5 P2 C7 104.50(9) . .
O2 P3 C13 105.66(9) 2_666 .
O5 P3 O2 98.95(7) . 2_666
O5 P3 C13 103.44(9) . .
O6 P3 O2 113.61(8) . 2_666
O6 P3 O5 115.77(8) . .
O6 P3 C13 117.26(10) . .
P1 O2 P3 129.80(9) . 2_666
P2 O3 P1 129.50(9) . .
P3 O5 P2 133.49(9) . .
C2 C1 P1 118.90(17) . .
C2 C1 C6 119.8(2) . .
C6 C1 P1 121.31(17) . .
C1 C2 H2 120.2 . .
C3 C2 C1 119.6(2) . .
C3 C2 H2 120.2 . .
C2 C3 H3 119.8 . .
C4 C3 C2 120.3(2) . .
C4 C3 H3 119.8 . .
C3 C4 H4 120.0 . .
C3 C4 C5 120.1(2) . .
C5 C4 H4 120.0 . .
C4 C5 H5 119.7 . .
C6 C5 C4 120.6(2) . .
C6 C5 H5 119.7 . .
C1 C6 H6 120.2 . .
C5 C6 C1 119.5(2) . .
C5 C6 H6 120.2 . .
C8 C7 P2 118.59(17) . .
C8 C7 C12 120.2(2) . .
C12 C7 P2 121.09(16) . .
C7 C8 H8 120.2 . .
C9 C8 C7 119.6(2) . .
C9 C8 H8 120.2 . .
C8 C9 H9 120.1 . .
C10 C9 C8 119.9(2) . .
C10 C9 H9 120.1 . .
C9 C10 H10 119.4 . .
C9 C10 C11 121.1(2) . .
C11 C10 H10 119.4 . .
C10 C11 H11 120.2 . .
C10 C11 C12 119.7(2) . .
C12 C11 H11 120.2 . .
C7 C12 H12 120.2 . .
C11 C12 C7 119.6(2) . .
C11 C12 H12 120.2 . .
C14 C13 P3 116.99(17) . .
C18 C13 P3 123.38(17) . .
C18 C13 C14 119.6(2) . .
C13 C14 H14 120.0 . .
C15 C14 C13 120.0(2) . .
C15 C14 H14 120.0 . .
C14 C15 H15 120.0 . .
C16 C15 C14 119.9(2) . .
C16 C15 H15 120.0 . .
C15 C16 H16 119.9 . .
C17 C16 C15 120.2(2) . .
C17 C16 H16 119.9 . .
C16 C17 H17 119.6 . .
C16 C17 C18 120.8(2) . .
C18 C17 H17 119.6 . .
C13 C18 C17 119.5(2) . .
C13 C18 H18 120.3 . .
C17 C18 H18 120.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
P1 O1 1.4543(14) .
P1 O2 1.5978(14) .
P1 O3 1.6039(15) .
P1 C1 1.761(2) .
P2 O3 1.6015(14) .
P2 O4 1.4511(15) .
P2 O5 1.6024(14) .
P2 C7 1.765(2) .
P3 O2 1.6053(15) 2_666
P3 O5 1.5922(14) .
P3 O6 1.4540(15) .
P3 C13 1.766(2) .
O2 P3 1.6053(15) 2_666
C1 C2 1.393(3) .
C1 C6 1.400(3) .
C2 H2 0.9500 .
C2 C3 1.387(3) .
C3 H3 0.9500 .
C3 C4 1.378(3) .
C4 H4 0.9500 .
C4 C5 1.381(3) .
C5 H5 0.9500 .
C5 C6 1.377(3) .
C6 H6 0.9500 .
C7 C8 1.392(3) .
C7 C12 1.393(3) .
C8 H8 0.9500 .
C8 C9 1.389(3) .
C9 H9 0.9500 .
C9 C10 1.372(3) .
C10 H10 0.9500 .
C10 C11 1.384(3) .
C11 H11 0.9500 .
C11 C12 1.387(3) .
C12 H12 0.9500 .
C13 C14 1.393(3) .
C13 C18 1.377(3) .
C14 H14 0.9500 .
C14 C15 1.385(3) .
C15 H15 0.9500 .
C15 C16 1.374(4) .
C16 H16 0.9500 .
C16 C17 1.361(4) .
C17 H17 0.9500 .
C17 C18 1.392(3) .
C18 H18 0.9500 .
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
1 0.000 0.500 0.000 177.8 41.7
