Crystal structure of catena{(μ2-1,10-phenanthroline-κ4 N,N,N′,N′)-(μ2-1,10-phenanthroline-κ3 N,N,N′)potassium(I) {[bis(2-hydroxyethyl)iminiumyl](sulfanidyl)methyl}sulfanide hemi(1,10-phenanthroline)}, {C24H16KN4, 0.5(C12H8N2), C5H10NO2S2}
Lo, Kong Mun; Lee, See Mun; Tiekink, Edward R.T.; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 1395–1397; doi:10.1515/ncrs-2020-0333

data_8105476
_publ_section_title
;
 Crystal structure of catena{(\m2-1,10-phenanthroline-\k4
 N,N,N&#x2032;,N&#x2032;)-(\m2-1,10-phenanthroline-\k3
 N,N,N&#x2032;)potassium(I)
 {[bis(2-hydroxyethyl)iminiumyl](sulfanidyl)methyl}sulfanide
 hemi(1,10-phenanthroline)}, {C24H16KN4, 0.5(C12H8N2), C5H10NO2S2}
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1395
_journal_page_last               1397
_journal_paper_doi               10.1515/ncrs-2020-0333
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C24 H16 K N4, 0.5(C12 H8 N2), C5 H10 N O2 S2'
_chemical_formula_sum            'C35 H30 K N6 O2 S2'
_chemical_formula_weight         669.87
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 94.3850(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.8001(4)
_cell_length_b                   7.15620(10)
_cell_length_c                   26.0400(3)
_cell_measurement_reflns_used    44499
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.3780
_cell_measurement_theta_min      5.4000
_cell_volume                     6094.32(13)
_computing_cell_refinement       'CrysAlisPro [1]'
_computing_data_collection       'CrysAlisPro [1]'
_computing_data_reduction        'CrysAlisPro [1]'
_computing_molecular_graphics    'ORTEP-3 for Windows [4]'
_computing_publication_material  'SHELXL-2018/3 [3]'
_computing_structure_refinement  'SHELXL-2018/3 [3]'
_computing_structure_solution    'SHELXT 2014/5 [2]'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2558
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0119
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            68443
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.074
_diffrn_reflns_theta_max         67.074
_diffrn_reflns_theta_min         3.404
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    3.170
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.805
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'CrysAlisPro [1]'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_description       prism
_exptl_crystal_F_000             2792
_exptl_crystal_size_max          0.132
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.039
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         5436
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0315
_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^)+(0.0372P)^2^+17.8982P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.0911
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5312
_reflns_number_total             5436
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2020-0333_suppl.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               8105476
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.680
_shelx_estimated_absorpt_t_max   0.886