Coordination chemistry of nitrile-functionalized mixed thia-aza macrocycles [9]aneN~2~S and [9]aneNS~2~ towards silver(I)
Blake, Alexander J.; Lippolis, Vito; Schroder, Martin; Acta Crystallographica Section C 78 (2022) –; doi:10.1107/S205322962200105X

data_2022548
_publ_section_title
;
 Coordination chemistry of nitrile-functionalized mixed thia-aza
 macrocycles [9]aneN~2~S and [9]aneNS~2~ towards silver(I)
;
_journal_coeditor_code           KY3213
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S205322962200105X
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac          '[Ag2 (C9 H16 N2 S2)2 (S C N)] B F4'
_chemical_formula_moiety         'C19 H32 Ag2 N5 S5 +, B F4 -'
_chemical_formula_sum            'C19 H32 Ag2 B F4 N5 S5'
_chemical_formula_weight         793.34
_chemical_name_systematic
'\m-Thiocyanato-\k^2^<i>S</i>:<i>S</i>-bis{[7-(2-cyanoethyl)-1,4-dithia-7-azacyclononane-\k^3^<i>N</i>,<i>S</i>,<i>S</i>']silver(I)} tetrafluoridoborate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 119.940(9)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.537(3)
_cell_length_b                   8.4362(11)
_cell_length_c                   27.216(3)
_cell_measurement_reflns_used    35
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      15.4
_cell_measurement_theta_min      11.1
_cell_volume                     5677.7(12)
_computing_cell_refinement
;
STADI-4 (Stoe & Cie, 1996)
;
_computing_data_collection
;
STADI-4 (Stoe & Cie, 1996)
;
_computing_data_reduction
;
X-RED (Stoe & Cie, 1996)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>, 2009) and Mercury (Macrae <i>et al.</i>,
2020)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>, 2009)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Stoe STADI4 4-circle'
_diffrn_measurement_method
; Scan width (omega) = 1.04 - 1.20, scan ratio 2theta:omega = 1.00
  I(Net) and sigma(I) calculated according to Blessing (1987)
;
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            5547
_diffrn_reflns_theta_full        24.983
_diffrn_reflns_theta_max         24.983
_diffrn_reflns_theta_min         2.551
_diffrn_standards_decay_%        7.0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.794
_exptl_absorpt_correction_T_max  0.8222
_exptl_absorpt_correction_T_min  0.7129
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
(SHELXTL; Sheldrick, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.856
_exptl_crystal_description       tablet
_exptl_crystal_F_000             3168
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.559
_refine_diff_density_min         -0.521
_refine_ls_extinction_coef       0.000099(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2018 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         4972
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0150P)^2^+34.6966P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0751
_reflns_number_gt                4138
_reflns_number_total             4972
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ky3213sup1.cif
_cod_data_source_block           Ag2L32mu-SCNBF4
_cod_original_cell_volume        5677.6(12)
_cod_database_code               2022548
_shelx_estimated_absorpt_t_min   0.643
_shelx_estimated_absorpt_t_max   0.814
_shelx_hkl_checksum              57732
_shelx_res_checksum              64592
_cod_database_fobs_code 2022548