Oxychloridoselenites(IV) with cubane-derived anions and stepwise chlorine-to-oxygen exchange.
Bonnin, Maxime A.; Feldmann, Claus; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d3dt01424j

data_7713300
_publ_section_title
;
 Oxychloridoselenites(IV) with cubane-derived anions and stepwise
 chlorine-to-oxygen exchange.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d3dt01424j
_journal_year                    2023
_chemical_formula_moiety         '2(Cl4 Se), 4(Cl2 O Se), 2(Cl), 2(C9 H20 N)'
_chemical_formula_sum            'C18 H40 Cl18 N2 O4 Se6'
_chemical_formula_weight         1460.38
_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
_audit_creation_date             2023-04-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-04-26 deposited with the CCDC.	2023-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                67.258(12)
_cell_angle_beta                 68.592(12)
_cell_angle_gamma                87.254(14)
_cell_formula_units_Z            1
_cell_length_a                   9.9777(17)
_cell_length_b                   10.5576(18)
_cell_length_c                   13.801(2)
_cell_measurement_reflns_used    12374
_cell_measurement_temperature    213
_cell_measurement_theta_max      28.93
_cell_measurement_theta_min      1.91
_cell_volume                     1240.9(4)
_computing_cell_refinement       'STOE X-Area'
_computing_data_collection       'STOE X-Area'
_computing_data_reduction        'STOE X-Area'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      213.0
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
 360 frames, detector distance = 100 mm
;
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14038
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         1.727
_exptl_absorpt_coefficient_mu    5.421
_exptl_absorpt_correction_T_max  0.1233
_exptl_absorpt_correction_T_min  0.0680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens in: F. R. Ahmed (Editor), "Crystallographic Computing", Munksgaard,
Copenhagen (1970), 255 - 270. Afterwards scaling of reflection intensities was
performed within STOE LANA. J. Koziskova, F. Hahn, J. Richter, J. Kozisek, Acta
Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Finally a spherical absorption correction was done within STOE LANA.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.954
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.570
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.902
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         4311
_refine_ls_number_restraints     349
_refine_ls_restrained_S_all      0.911
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0266
_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^)+(0.0386P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0598
_refine_ls_wR_factor_ref         0.0628
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3216
_reflns_number_total             4311
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01424j2.cif
_cod_data_source_block           5
_cod_database_code               7713300
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.671
_shelx_estimated_absorpt_t_min   0.587
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Se3B-O2B \\sim Se3A-O2A \\sim Se1-O1
 with sigma of 0.02
 C5B-C6B \\sim C5A-C6A
 with sigma of 0.04
 C6B-C8B \\sim C6A-C8A
 with sigma of 0.04
 C7B-C9B \\sim C7A-C9A
 with sigma of 0.04
 C8B-C9B \\sim C8A-C9A
 with sigma of 0.02
 C5B-C4B \\sim C5A-C4A
 with sigma of 0.02
 C6B-C7B \\sim C6A-C7A \\sim C7B-C8B \\sim C7A-C8A
 with sigma of 0.02
 N1B-C1B \\sim N1A-C1A
 with sigma of 0.02
 N1B-C2B \\sim N1A-C2A \\sim N1B-C5B \\sim N1A-C5A \\sim N1B-C6B \\sim N1A-C6A
 with sigma of 0.02
 N1B-C3B \\sim N1A-C3A
 with sigma of 0.04
 N1B-C4B \\sim N1A-C4A
 with sigma of 0.04
 N1B-C7B \\sim N1A-C7A
 with sigma of 0.04
 C1B-C2B \\sim C1A-C2A
 with sigma of 0.04
 C1B-C5B \\sim C1A-C5A
 with sigma of 0.04
 C1B-C6B \\sim C1A-C6A
 with sigma of 0.04
 C2B-C3B \\sim C2A-C3A
 with sigma of 0.02
 C2B-C5B \\sim C2A-C5A
 with sigma of 0.04
 C2B-C4B \\sim C2A-C4A
 with sigma of 0.04
 C2B-C6B \\sim C2A-C6A
 with sigma of 0.04
 C2B-C7B \\sim C2A-C7A
 with sigma of 0.04
 C3B-C5B \\sim C3A-C5A
 with sigma of 0.04
 C3B-C4B \\sim C3A-C4A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1B \\sim C8A \\sim C6A \\sim C2B \\sim C2A \\sim C3B \\sim C4A \\sim C5B \\sim
N1B \\sim C4B \\sim C5A \\sim C6B \\sim C3A \\sim C7B \\sim C7A \\sim C8B \\sim
C9A \\sim C9B \\sim N1A \\sim C1A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
4. Others
 Sof(N1A)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=
 Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(C3A)=Sof(H3AA)=
 Sof(H3AB)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(C8A)=
 Sof(H8AA)=Sof(H8AB)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=1-FVAR(1)
 Sof(N1B)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=
 Sof(C3B)=Sof(H3BA)=Sof(H3BB)=Sof(C5B)=Sof(H5BA)=Sof(H5BB)=Sof(C4B)=Sof(H4BA)=
 Sof(H4BB)=Sof(C6B)=Sof(H6BA)=Sof(H6BB)=Sof(C7B)=Sof(H7BA)=Sof(H7BB)=Sof(C8B)=
 Sof(H8BA)=Sof(H8BB)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(H9BC)=FVAR(1)
 Fixed Sof: Se3A(0.5) Cl9A(0.5) O2A(0.5) Cl8A(0.5) Se3B(0.5) Cl8B(0.5)
 O2B(0.5) Cl9B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C2B(H2BA,H2BB), C3B(H3BA,H3BB), C5B(H5BA,H5BB), C4B(H4BA,H4BB), C6B(H6BA,
 H6BB), C7B(H7BA,H7BB), C8B(H8BA,H8BB), C2A(H2AA,H2AB), C5A(H5AA,H5AB),
 C6A(H6AA,H6AB), C3A(H3AA,H3AB), C4A(H4AA,H4AB), C7A(H7AA,H7AB), C8A(H8AA,H8AB)
5.b Idealised Me refined as rotating group:
 C1B(H1BA,H1BB,H1BC), C9B(H9BA,H9BB,H9BC), C1A(H1AA,H1AB,H1AC), C9A(H9AA,H9AB,
 H9AC)
;
_shelx_res_checksum              60611
_olex2_submission_special_instructions 'No special instructions were received'