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_7124520
_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/[\s^2^(Fo^2^)+(0.0193P)^2^+8.9124P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(I)'
_cod_data_source_file            c9cc08347b2.cif
_cod_data_source_block           li0394
_cod_database_code               7124520
_shelx_shelxl_version_number     2018/3
_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)
;
_shelx_res_checksum              86248
_olex2_submission_special_instructions 'No special instructions were received'