Catenated and Spirocyclic Polychalcogenides from Potassium Carbonate and Elemental Chalcogens
Chivers, Tristram; Edelmann, Frank T.; Liebing , Phil; Hilfert, Liane; Goldhahn , R.; Feneberg, Martin; Swanson, Claudia; kueling, marcel; Chemical Communications  (2019) –; doi:10.1039/C9CC08347B

data_7124519
_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_absolute_configuration ad
_chemical_formula_moiety         'S12, 2(C36 H30 N P2)'
_chemical_formula_sum            'C72 H60 N2 P4 S12'
_chemical_formula_weight         1461.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-07-02
_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                 95.642(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6600(3)
_cell_length_b                   14.2151(3)
_cell_length_c                   35.8526(9)
_cell_measurement_reflns_used    16543
_cell_measurement_temperature    133.15
_cell_measurement_theta_max      25.104
_cell_measurement_theta_min      2.073
_cell_volume                     6928.1(3)
_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 0.962
_diffrn_measured_fraction_theta_max 0.962
_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  0.0219
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            16543
_diffrn_reflns_point_group_measured_fraction_full 0.772
_diffrn_reflns_point_group_measured_fraction_max 0.772
_diffrn_reflns_theta_full        25.104
_diffrn_reflns_theta_max         25.104
_diffrn_reflns_theta_min         2.073
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.516
_exptl_absorpt_correction_T_max  0.9411
_exptl_absorpt_correction_T_min  0.8670
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Area and X-Red (STOE & Cie, 2018/12)'
_exptl_crystal_colour            'dark violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_description       prism
_exptl_crystal_F_000             3032
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.732
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.34(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     812
_refine_ls_number_reflns         9530
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0351
_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/[\s^2^(Fo^2^)+(0.0405P)^2^+16.9361P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0879
_reflns_Friedel_coverage         0.605
_reflns_Friedel_fraction_full    0.582
_reflns_Friedel_fraction_max     0.582
_reflns_number_gt                9065
_reflns_number_total             9530
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc08347b2.cif
_cod_data_source_block           li0388
_cod_database_code               7124519
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.832
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.66(7)
 0.34(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.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), 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), C38(H38), C39(H39),
  C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47),
 C48(H48), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C56(H56), C57(H57),
  C58(H58), C59(H59), C60(H60), C62(H62), C63(H63), C64(H64), C65(H65),
 C66(H66), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72)
;
_shelx_res_checksum              56290
_olex2_submission_special_instructions 'No special instructions were received'