#------------------------------------------------------------------------------
#$Date: 2019-11-20 03:47:22 +0200 (Wed, 20 Nov 2019) $
#$Revision: 231063 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/45/7124520.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_7124520
loop_
_publ_author_name
'Chivers, Tristram'
'Edelmann, Frank T.'
'Liebing , Phil'
'Hilfert, Liane'
'Goldhahn , R.'
'Feneberg, Martin'
'Swanson, Claudia'
'kueling, marcel'
_publ_section_title
;
 Catenated and Spirocyclic Polychalcogenides from Potassium Carbonate and
 Elemental Chalcogens
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC08347B
_journal_year                    2019
_chemical_formula_moiety         'Se11, 2(C36 H30 N P2)'
_chemical_formula_sum            'C72 H60 N2 P4 Se11'
_chemical_formula_weight         1945.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-07-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-16 deposited with the CCDC.	2019-11-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.713(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.9704(3)
_cell_length_b                   18.3061(4)
_cell_length_c                   17.7630(5)
_cell_measurement_reflns_used    26598
_cell_measurement_temperature    133.15
_cell_measurement_theta_max      29.240
_cell_measurement_theta_min      2.172
_cell_volume                     3549.54(16)
_computing_cell_refinement       'X-Area (STOE & Cie, 2018/12)'
_computing_data_collection       'X-Area (STOE & Cie, 2018/12)'
_computing_data_reduction        'X-Area and X-Red (STOE & Cie, 2018/12)'
_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      133.15
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            26598
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.240
_diffrn_reflns_theta_min         2.172
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.790
_exptl_absorpt_correction_T_max  0.4328
_exptl_absorpt_correction_T_min  0.3375
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'X-Area, X-Red and X-Shape (STOE & Cie, 2018/12)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.820
_exptl_crystal_description       prism
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.945
_refine_diff_density_min         -0.914
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         9545
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0439
_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)+(0.0193P)²+8.9124P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0872
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7086
_reflns_number_total             9545
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9cc08347b2.cif
_cod_data_source_block           li0394
_cod_database_code               7124520
_shelx_shelxl_version_number     2018/3
_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   0.349
_shelx_estimated_absorpt_t_min   0.211
_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), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29),
 C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, 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
Se1 Se 0.000000 0.500000 0.500000 0.02899(13) Uani 1 2 d S T P
Se2 Se -0.04515(5) 0.44280(3) 0.36321(2) 0.04195(12) Uani 1 1 d . . .
Se3 Se -0.00237(4) 0.31973(2) 0.37539(2) 0.03438(10) Uani 1 1 d . . .
Se4 Se -0.16414(4) 0.26614(3) 0.43258(3) 0.05045(15) Uani 1 1 d . . .
Se5 Se -0.12664(5) 0.30630(3) 0.55788(3) 0.04613(13) Uani 1 1 d . . .
Se6 Se -0.18132(4) 0.42834(3) 0.55637(2) 0.03258(10) Uani 1 1 d . . .
P1 P 0.39500(7) 0.17614(4) 0.37615(4) 0.01328(15) Uani 1 1 d . . .
P2 P 0.39655(7) 0.16700(4) 0.54431(4) 0.01371(15) Uani 1 1 d . . .
N1 N 0.4044(3) 0.14495(15) 0.45931(15) 0.0171(5) Uani 1 1 d . . .
C1 C 0.5180(3) 0.13863(18) 0.32853(17) 0.0146(6) Uani 1 1 d . . .
C2 C 0.5320(3) 0.06262(19) 0.32928(19) 0.0206(7) Uani 1 1 d . . .
H2 H 0.476813 0.032811 0.353535 0.025 Uiso 1 1 calc R . .
C3 C 0.6261(3) 0.0311(2) 0.29475(19) 0.0215(7) Uani 1 1 d . . .
H3 H 0.635345 -0.020473 0.294888 0.026 Uiso 1 1 calc R . .
C4 C 0.7073(3) 0.0746(2) 0.25983(19) 0.0206(7) Uani 1 1 d . . .
H4 H 0.772329 0.052658 0.236469 0.025 Uiso 1 1 calc R . .
C5 C 0.6943(3) 0.1496(2) 0.25873(19) 0.0215(7) Uani 1 1 d . . .
H5 H 0.749817 0.179091 0.234417 0.026 Uiso 1 1 calc R . .
C6 C 0.5994(3) 0.18173(19) 0.29339(18) 0.0189(6) Uani 1 1 d . . .
H6 H 0.590470 0.233346 0.292968 0.023 Uiso 1 1 calc R . .
C7 C 0.4036(3) 0.27372(17) 0.37115(17) 0.0152(6) Uani 1 1 d . . .
C8 C 0.5047(3) 0.30858(19) 0.40875(19) 0.0200(7) Uani 1 1 d . . .
H8 H 0.570456 0.280494 0.432600 0.024 Uiso 1 1 calc R . .
C9 C 0.5097(3) 0.3838(2) 0.4115(2) 0.0237(7) Uani 1 1 d . . .
H9 H 0.579400 0.407567 0.436417 0.028 Uiso 1 1 calc R . .
C10 C 0.4125(3) 0.4248(2) 0.3775(2) 0.0266(8) Uani 1 1 d . . .
H10 H 0.415234 0.476643 0.380457 0.032 Uiso 1 1 calc R . .
C11 C 0.3120(3) 0.3908(2) 0.3396(2) 0.0241(7) Uani 1 1 d . . .
H11 H 0.246486 0.419147 0.315980 0.029 Uiso 1 1 calc R . .
C12 C 0.3069(3) 0.31504(19) 0.33597(18) 0.0185(6) Uani 1 1 d . . .
H12 H 0.238192 0.291445 0.309754 0.022 Uiso 1 1 calc R . .
C13 C 0.2459(3) 0.1392(2) 0.24670(19) 0.0239(7) Uani 1 1 d . . .
H13 H 0.317121 0.143064 0.220616 0.029 Uiso 1 1 calc R . .
C14 C 0.1327(3) 0.1234(2) 0.2071(2) 0.0314(9) Uani 1 1 d . . .
H14 H 0.126954 0.115538 0.153969 0.038 Uiso 1 1 calc R . .
C15 C 0.0290(3) 0.1192(2) 0.2451(2) 0.0274(8) Uani 1 1 d . . .
H15 H -0.047915 0.108838 0.217738 0.033 Uiso 1 1 calc R . .
C16 C 0.0360(3) 0.1298(2) 0.3221(2) 0.0226(7) Uani 1 1 d . . .
H16 H -0.035955 0.127124 0.347609 0.027 Uiso 1 1 calc R . .
C17 C 0.1478(3) 0.14436(19) 0.36233(18) 0.0187(6) Uani 1 1 d . . .
H17 H 0.152722 0.151056 0.415582 0.022 Uiso 1 1 calc R . .
C18 C 0.2537(3) 0.14925(17) 0.32471(18) 0.0160(6) Uani 1 1 d . . .
C19 C 0.5313(3) 0.13471(17) 0.59967(17) 0.0155(6) Uani 1 1 d . . .
C20 C 0.5391(3) 0.13468(18) 0.67871(18) 0.0191(7) Uani 1 1 d . . .
H20 H 0.471043 0.149792 0.703965 0.023 Uiso 1 1 calc R . .
C21 C 0.6466(3) 0.1125(2) 0.7201(2) 0.0273(8) Uani 1 1 d . . .
H21 H 0.651948 0.112125 0.773824 0.033 Uiso 1 1 calc R . .
C22 C 0.7456(4) 0.0911(3) 0.6836(2) 0.0380(10) Uani 1 1 d . . .
H22 H 0.818827 0.075703 0.712259 0.046 Uiso 1 1 calc R . .
C23 C 0.7389(4) 0.0917(3) 0.6054(2) 0.0439(12) Uani 1 1 d . . .
H23 H 0.807913 0.077324 0.580634 0.053 Uiso 1 1 calc R . .
C24 C 0.6319(3) 0.1134(2) 0.5630(2) 0.0287(8) Uani 1 1 d . . .
H24 H 0.627355 0.113592 0.509343 0.034 Uiso 1 1 calc R . .
C25 C 0.2655(3) 0.12397(18) 0.57835(17) 0.0161(6) Uani 1 1 d . . .
C26 C 0.2284(3) 0.05615(19) 0.5484(2) 0.0224(7) Uani 1 1 d . . .
H26 H 0.269995 0.034723 0.509476 0.027 Uiso 1 1 calc R . .
C27 C 0.1306(3) 0.0201(2) 0.5756(2) 0.0263(8) Uani 1 1 d . . .
H27 H 0.104780 -0.025801 0.554831 0.032 Uiso 1 1 calc R . .
C28 C 0.0705(3) 0.0507(2) 0.6326(2) 0.0287(8) Uani 1 1 d . . .
H28 H 0.004462 0.025232 0.651587 0.034 Uiso 1 1 calc R . .
C29 C 0.1059(3) 0.1181(2) 0.6623(2) 0.0283(8) Uani 1 1 d . . .
H29 H 0.063752 0.139211 0.701085 0.034 Uiso 1 1 calc R . .
C30 C 0.2034(3) 0.1547(2) 0.63523(19) 0.0226(7) Uani 1 1 d . . .
H30 H 0.227781 0.201065 0.655598 0.027 Uiso 1 1 calc R . .
C31 C 0.3842(3) 0.26276(17) 0.56149(17) 0.0148(6) Uani 1 1 d . . .
C32 C 0.2772(3) 0.29890(19) 0.53180(18) 0.0191(7) Uani 1 1 d . . .
H32 H 0.210481 0.271681 0.507918 0.023 Uiso 1 1 calc R . .
C33 C 0.2689(3) 0.3735(2) 0.5372(2) 0.0244(7) Uani 1 1 d . . .
H33 H 0.197412 0.398153 0.515840 0.029 Uiso 1 1 calc R . .
C34 C 0.3651(4) 0.4127(2) 0.5739(2) 0.0287(8) Uani 1 1 d . . .
H34 H 0.358568 0.464223 0.578484 0.034 Uiso 1 1 calc R . .
C35 C 0.4703(4) 0.3778(2) 0.6039(2) 0.0257(8) Uani 1 1 d . . .
H35 H 0.535326 0.405320 0.629283 0.031 Uiso 1 1 calc R . .
C36 C 0.4814(3) 0.30265(18) 0.59712(18) 0.0188(6) Uani 1 1 d . . .
H36 H 0.554606 0.278673 0.616606 0.023 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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 '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
Se2 Se1 Se2 180.0 3_566 .
Se2 Se1 Se6 85.880(15) 3_566 .
Se2 Se1 Se6 94.120(15) . .
Se2 Se1 Se6 85.882(15) . 3_566
Se2 Se1 Se6 94.118(15) 3_566 3_566
Se6 Se1 Se6 180.0 3_566 .
Se3 Se2 Se1 106.409(19) . .
Se2 Se3 Se4 107.06(2) . .
Se5 Se4 Se3 102.21(2) . .
Se6 Se5 Se4 105.75(3) . .
Se5 Se6 Se1 106.136(19) . .
N1 P1 C1 108.66(15) . .
N1 P1 C7 114.11(15) . .
N1 P1 C18 110.58(15) . .
C7 P1 C1 108.16(15) . .
C18 P1 C1 107.90(15) . .
C18 P1 C7 107.24(15) . .
N1 P2 C19 108.70(15) . .
N1 P2 C25 109.43(15) . .
N1 P2 C31 115.34(14) . .
C19 P2 C25 108.35(15) . .
C31 P2 C19 107.59(15) . .
C31 P2 C25 107.22(15) . .
P2 N1 P1 143.21(19) . .
C2 C1 P1 117.5(2) . .
C6 C1 P1 122.8(3) . .
C6 C1 C2 119.7(3) . .
C3 C2 C1 119.9(3) . .
C2 C3 C4 120.1(3) . .
C5 C4 C3 120.5(3) . .
C4 C5 C6 119.7(3) . .
C1 C6 C5 120.1(3) . .
C8 C7 P1 118.5(2) . .
C8 C7 C12 120.0(3) . .
C12 C7 P1 121.3(2) . .
C9 C8 C7 120.1(3) . .
C8 C9 C10 119.9(3) . .
C11 C10 C9 120.5(3) . .
C10 C11 C12 120.0(3) . .
C11 C12 C7 119.6(3) . .
C18 C13 C14 119.6(3) . .
C15 C14 C13 120.0(3) . .
C16 C15 C14 120.7(3) . .
C15 C16 C17 120.0(3) . .
C16 C17 C18 120.1(3) . .
C13 C18 P1 120.6(2) . .
C13 C18 C17 119.6(3) . .
C17 C18 P1 119.5(2) . .
C20 C19 P2 121.0(2) . .
C24 C19 P2 119.0(2) . .
C24 C19 C20 119.8(3) . .
C21 C20 C19 119.8(3) . .
C22 C21 C20 120.2(3) . .
C21 C22 C23 120.4(4) . .
C22 C23 C24 120.3(4) . .
C23 C24 C19 119.6(3) . .
C26 C25 P2 118.4(2) . .
C30 C25 P2 122.2(3) . .
C30 C25 C26 119.4(3) . .
C27 C26 C25 119.8(3) . .
C28 C27 C26 120.4(4) . .
C27 C28 C29 120.2(3) . .
C28 C29 C30 119.8(3) . .
C29 C30 C25 120.3(3) . .
C32 C31 P2 118.2(2) . .
C36 C31 P2 121.7(2) . .
C36 C31 C32 119.8(3) . .
C33 C32 C31 120.1(3) . .
C32 C33 C34 119.7(3) . .
C35 C34 C33 120.8(3) . .
C34 C35 C36 120.2(3) . .
C35 C36 C31 119.3(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Se1 Se2 2.6469(4) 3_566
Se1 Se2 2.6470(4) .
Se1 Se6 2.6601(4) 3_566
Se1 Se6 2.6602(4) .
Se2 Se3 2.3070(7) .
Se3 Se4 2.3458(7) .
Se4 Se5 2.3411(7) .
Se5 Se6 2.3128(7) .
P1 N1 1.577(3) .
P1 C1 1.799(3) .
P1 C7 1.791(3) .
P1 C18 1.788(3) .
P2 N1 1.574(3) .
P2 C19 1.793(3) .
P2 C25 1.796(3) .
P2 C31 1.787(3) .
C1 C2 1.400(5) .
C1 C6 1.386(4) .
C2 C3 1.378(5) .
C3 C4 1.386(5) .
C4 C5 1.379(5) .
C5 C6 1.391(5) .
C7 C8 1.392(4) .
C7 C12 1.398(4) .
C8 C9 1.379(5) .
C9 C10 1.392(5) .
C10 C11 1.382(5) .
C11 C12 1.389(5) .
C13 C14 1.395(5) .
C13 C18 1.392(4) .
C14 C15 1.381(5) .
C15 C16 1.377(5) .
C16 C17 1.382(5) .
C17 C18 1.400(4) .
C19 C20 1.398(4) .
C19 C24 1.392(5) .
C20 C21 1.387(5) .
C21 C22 1.376(5) .
C22 C23 1.384(6) .
C23 C24 1.388(5) .
C25 C26 1.395(5) .
C25 C30 1.393(5) .
C26 C27 1.386(5) .
C27 C28 1.381(5) .
C28 C29 1.382(6) .
C29 C30 1.388(5) .
C31 C32 1.403(4) .
C31 C36 1.391(4) .
C32 C33 1.373(5) .
C33 C34 1.384(5) .
C34 C35 1.378(5) .
C35 C36 1.388(5) .
