Copper(II) Prevents the Saccarine-Dialkylcyanamide Coupling by Forming Mononuclear (Saccharinate)(Dialkylcyanamide)copper(II) Complexes
Toikka, Yulia N.; Spiridonova, Dar’ya V.; Novikov, Alexander S.; Bokach, Nadezhda A.; Inorganics 9 (2021) 69–; doi:10.3390/inorganics9090069

data_1564851
_publ_section_title
;
 Copper(II) Prevents the Saccarine-Dialkylcyanamide Coupling by Forming
 Mononuclear (Saccharinate)(Dialkylcyanamide)copper(II) Complexes
;
_journal_issue                   9
_journal_name_full               Inorganics
_journal_page_first              69
_journal_paper_doi               10.3390/inorganics9090069
_journal_volume                  9
_journal_year                    2021
_chemical_formula_moiety         'C17 H18 Cu N4 O8 S2'
_chemical_formula_sum            'C17 H18 Cu N4 O8 S2'
_chemical_formula_weight         534.01
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.14100(10)
_cell_length_b                   23.8599(4)
_cell_length_c                   12.48922(19)
_cell_measurement_reflns_used    5013
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.2150
_cell_measurement_theta_min      1.8630
_cell_volume                     2127.96(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -62.00 -12.00   0.50    0.20    --  -38.82  97.00-113.00  100
  2  \w     -1.00  30.00   0.50    0.20    --  -38.82  27.00 111.00   62
  3  \w    -47.00  -6.00   0.50    0.20    --  -38.82  27.00 111.00   82
  4  \w    -72.00 -37.00   0.50    0.20    --  -38.82 122.00 -34.00   70
  5  \w     77.00 102.00   0.50    0.20    --   38.82  27.00 111.00   50
  6  \w     18.00  58.00   0.50    0.20    --   38.82-150.00  82.00   80
  7  \w     24.00  49.00   0.50    0.20    --   38.82  27.00 111.00   50
  8  \w     33.00  59.00   0.50    0.20    --   38.82 -97.00 139.00   52
  9  \w     31.00  63.00   0.50    0.20    --   38.82-122.00-115.00   64
 10  \w    -29.00  -3.00   0.50    0.20    --   38.82 -27.00 -51.00   52
 11  \w     85.00 147.00   0.50    0.20    --  100.00  97.00-113.00  124
 12  \w     31.00  72.00   0.50    0.20    --  100.00 -27.00 -51.00   82
 13  \w    110.00 136.00   0.50    0.20    --  100.00  27.00 111.00   52
 14  \w     69.00  94.00   0.50    0.20    --  100.00-122.00-115.00   50
 15  \w     60.00  93.00   0.50    0.20    --  100.00 -97.00 139.00   66
 16  \w     85.00 110.00   0.50    0.20    --  100.00 150.00 127.00   50
 17  \w   -104.00 -51.00   0.50    0.20    --  -38.82 -21.00 120.00  106
 18  \w    -90.00 -65.00   0.50    0.20    --  -38.82 -27.00 -51.00   50
 19  \w     56.00  81.00   0.50    0.20    --   38.82  54.00-120.00   50
 20  \w    -18.00   8.00   0.50    0.20    --   38.82 -43.00-150.00   52
 21  \w     15.00  55.00   0.50    0.20    --   38.82 -43.00-150.00   80
 22  \w     89.00 115.00   0.50    0.20    --  100.00  37.00-120.00   52
 23  \w     55.00  83.00   0.50    0.20    --  100.00-111.00  60.00   56
 24  \w     84.00 156.00   0.50    0.20    --  100.00 111.00   0.00  144
 25  \w     70.00 155.00   0.50    0.20    --  100.00  15.00   0.00  170
 26  \w     34.00 125.00   0.50    0.20    --  100.00 -69.00-180.00  182
 27  \w     36.00  80.00   0.50    0.20    --  100.00-133.00 150.00   88
 28  \w     36.00  82.00   0.50    0.20    --  100.00-133.00-150.00   92
 29  \w    104.00 157.00   0.50    0.20    --  100.00  93.00  30.00  106
 30  \w     77.00 108.50   0.50    0.20    --  100.00-150.00  82.00   63
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0649740000
_diffrn_orient_matrix_UB_12      -0.0593066000
_diffrn_orient_matrix_UB_13      -0.0314768000
_diffrn_orient_matrix_UB_21      0.0383342000
_diffrn_orient_matrix_UB_22      -0.0134764000
_diffrn_orient_matrix_UB_23      0.1186209000
_diffrn_orient_matrix_UB_31      -0.2021595000
_diffrn_orient_matrix_UB_32      -0.0216383000
_diffrn_orient_matrix_UB_33      0.0124252000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7905
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.944
_diffrn_reflns_theta_min         3.705
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.773
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77050
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_description       prism
_exptl_crystal_F_000             1092
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2068
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0338
_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^)+(0.0532P)^2^+1.6018P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.0951
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1919
_reflns_number_total             2068
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            YN44.cif
_cod_data_source_block           yn44
_cod_database_code               1564851
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Cu1 C16 N4 O2'
_shelx_estimated_absorpt_t_max   0.704
_shelx_estimated_absorpt_t_min   0.550
_reflns_odcompleteness_completeness 98.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     70.93
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6)
2.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C)
;
_shelx_res_checksum              90594
_shelx_hkl_checksum              48439
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.206
_oxdiff_exptl_absorpt_empirical_full_min 0.797