Snapshot and crystallographic observations of kinetic and thermodynamic products for NO<sub>2</sub>S<sub>2</sub> macrocyclic complexes.
Park, In-Hyeok; Kang, Yunji; Lee, Eunji; Ju, Huiyeong; Kim, Seulgi; Seo, Sujin; Jung, Jong Hwa; Lee, Shim Sung; IUCrJ 5 (2018) 45–53; doi:10.1107/S2052252517015081

data_1556832
_publ_section_title
;
 Snapshot and crystallographic observations of kinetic and thermodynamic
 products for NO<sub>2</sub>S<sub>2</sub> macrocyclic complexes.
;
_journal_issue                   'Pt 1'
_journal_name_full               IUCrJ
_journal_page_first              45
_journal_page_last               53
_journal_paper_doi               10.1107/S2052252517015081
_journal_volume                  5
_journal_year                    2018
_chemical_formula_sum            'C116 H106 Cd8 I16 N4 O8 S8'
_chemical_formula_weight         4870.12
_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_method           SHELXL-2014/7
_cell_angle_alpha                86.655(7)
_cell_angle_beta                 89.396(6)
_cell_angle_gamma                78.371(7)
_cell_formula_units_Z            1
_cell_length_a                   11.3166(11)
_cell_length_b                   13.4404(15)
_cell_length_c                   24.586(2)
_cell_measurement_reflns_used    7371
_cell_measurement_temperature    171(2)
_cell_measurement_theta_max      23.30
_cell_measurement_theta_min      2.15
_cell_volume                     3656.5(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      171(2)
_diffrn_measured_fraction_theta_full 0.802
_diffrn_measured_fraction_theta_max 0.802
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0842
_diffrn_reflns_av_unetI/netI     0.1217
_diffrn_reflns_Laue_measured_fraction_full 0.802
_diffrn_reflns_Laue_measured_fraction_max 0.802
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            23781
_diffrn_reflns_point_group_measured_fraction_full 0.802
_diffrn_reflns_point_group_measured_fraction_max 0.802
_diffrn_reflns_theta_full        23.253
_diffrn_reflns_theta_max         23.253
_diffrn_reflns_theta_min         2.632
_exptl_absorpt_coefficient_mu    4.680
_exptl_absorpt_correction_T_max  0.8348
_exptl_absorpt_correction_T_min  0.3539
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.212
_exptl_crystal_description       needle
_exptl_crystal_F_000             2254
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.040
_refine_diff_density_max         3.799
_refine_diff_density_min         -1.967
_refine_diff_density_rms         0.530
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         8432
_refine_ls_number_restraints     1058
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.2147
_refine_ls_R_factor_gt           0.1848
_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^)+(0.0399P)^2^+1891.6968P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4191
_refine_ls_wR_factor_ref         0.4304
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6056
_reflns_number_total             8432
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yc5012.cif
_cod_data_source_block           4
_cod_original_cell_volume        3656.6(6)
_cod_database_code               1556832
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.354
_shelx_estimated_absorpt_t_max   0.835
_shelx_hkl_checksum              40483
_shelx_fab_checksum              6549