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_7713298
_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         'Cl4 O Se, 2(C8 H15 N2)'
_chemical_formula_sum            'C16 H30 Cl4 N4 O Se'
_chemical_formula_weight         515.20
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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                73.69(3)
_cell_angle_beta                 72.73(3)
_cell_angle_gamma                63.57(3)
_cell_formula_units_Z            1
_cell_length_a                   8.570(4)
_cell_length_b                   8.857(4)
_cell_length_c                   9.228(4)
_cell_measurement_reflns_used    2363
_cell_measurement_temperature    213
_cell_measurement_theta_max      21.94
_cell_measurement_theta_min      2.27
_cell_volume                     589.8(5)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
 432 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  0.0810
_diffrn_reflns_av_unetI/netI     0.2234
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7614
_diffrn_reflns_point_group_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        24.993
_diffrn_reflns_theta_max         24.993
_diffrn_reflns_theta_min         2.347
_exptl_absorpt_coefficient_mu    2.057
_exptl_absorpt_correction_T_max  0.8483
_exptl_absorpt_correction_T_min  0.4542
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             264
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.229
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.40(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.608
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         3970
_refine_ls_number_restraints     579
_refine_ls_restrained_S_all      0.631
_refine_ls_R_factor_all          0.1160
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0236P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0867
_reflns_Friedel_coverage         0.909
_reflns_Friedel_fraction_full    0.909
_reflns_Friedel_fraction_max     0.909
_reflns_number_gt                1406
_reflns_number_total             3970
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01424j2.cif
_cod_data_source_block           6
_cod_original_cell_volume        589.9(5)
_cod_database_code               7713298
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.922
_shelx_estimated_absorpt_t_min   0.853
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.60(3)
 0.40(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
N2 \\sim N1 \\sim C4 \\sim C2 \\sim C1 \\sim H4 \\sim C3 \\sim H2 \\sim H1A
\\sim H1B \\sim H1C \\sim C5 \\sim H3 \\sim H5A \\sim H5B \\sim C6 \\sim H6A
\\sim H6B \\sim C7 \\sim C8 \\sim H7A \\sim H7B \\sim H8A \\sim H8B \\sim H8C
\\sim C15 \\sim N3 \\sim C10 \\sim C9 \\sim C12 \\sim H10 \\sim C11 \\sim H9A
\\sim H9B \\sim H9C \\sim N4 \\sim H12 \\sim H11 \\sim C13 \\sim C14 \\sim H13A
\\sim H13B \\sim H14A \\sim H14B \\sim H15A \\sim H15B \\sim C16 \\sim H16A
\\sim H16B \\sim H16C: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 C15, N3, C10, C9, C12, H10, C11, H9A, H9B, H9C, N4, H12, H11, C13, C14, H13A,
 H13B, H14A, H14B, H15A, H15B, C16, H16A, H16B, H16C, C5, N1, C4, C2, C1, H4,
 N2, C3, H2, H1A, H1B, H1C, H3, H5A, H5B, C6, H6A, H6B, C7, C8, H7A, H7B, H8A,
 H8B, H8C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C13(H13A,H13B), C5(H5A,H5B), C15(H15A,H15B), C6(H6A,H6B),
 C7(H7A,H7B)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), C10(H10), C11(H11), C2(H2), C12(H12)
5.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C1(H1A,H1B,H1C), C8(H8A,H8B,H8C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              90372
_olex2_submission_special_instructions 'No special instructions were received'