Rare proximity enforced copper hydrogen interactions in copper(i)-chalcogenones
Mannarsamy, Maruthupandi; Prabusankar, Ganesan; New Journal of Chemistry 45 (2021) 5933–5938; doi:10.1039/D1NJ00397F

data_7060433
_publ_section_title
;
 Rare proximity enforced copper hydrogen interactions in
 copper(i)-chalcogenones
;
_journal_issue                   13
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              5933
_journal_page_last               5938
_journal_paper_doi               10.1039/D1NJ00397F
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C22 H26 N4 S2'
_chemical_formula_sum            'C22 H26 N4 S2'
_chemical_formula_weight         410.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-12-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-12-04 deposited with the CCDC.	2021-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.344(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2395(6)
_cell_length_b                   15.3428(6)
_cell_length_c                   13.9990(6)
_cell_measurement_reflns_used    3123
_cell_measurement_temperature    298
_cell_measurement_theta_max      68.8190
_cell_measurement_theta_min      3.9740
_cell_volume                     2395.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      298.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1293
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9795
_diffrn_measured_fraction_theta_max 0.9795
_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    -69.00 -33.00   1.00    2.56    --    0.00 -57.00   0.00   36
  2  \w    -20.00   6.00   1.00    2.56    --    0.00  57.00 150.00   26
  3  \w      8.00  33.00   1.00    2.56    --    0.00  57.00 150.00   25
  4  \w    -13.00  14.00   1.00    2.56    --    0.00 -57.00   0.00   27
  5  \w     33.00 111.00   1.00   10.23    --   54.00  57.00-120.00   78
  6  \w     56.00  89.00   1.00   10.23    --   54.00-125.00-180.00   33
  7  \w     58.00 123.00   1.00   10.23    --   54.00  57.00 -60.00   65
  8  \w     24.00  68.00   1.00   10.23    --   54.00 -57.00   0.00   44
  9  \w    -15.00  39.00   1.00   10.23    --   54.00 -57.00 150.00   54
 10  \w     37.00 117.00   1.00   10.23    --  108.00 -77.00  60.00   80
 11  \w    100.00 174.00   1.00   10.23    --  108.00 111.00  90.00   74
 12  \w     98.00 133.00   1.00   10.23    --  108.00  77.00  90.00   35
 13  \w     36.00  95.00   1.00   10.23    --  108.00-111.00  30.00   59
 14  \w     46.00  94.00   1.00   10.23    --  108.00-111.00-150.00   48
 15  \w    123.00 178.00   1.00   10.23    --  108.00 111.00   0.00   55
 16  \w     71.00  97.00   1.00   10.23    --  108.00-111.00  60.00   26
 17  \w     84.00 172.00   1.00   10.23    --  108.00  63.00-150.00   88
 18  \w     84.00 175.00   1.00   10.23    --  108.00  63.00-180.00   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0592677000
_diffrn_orient_matrix_UB_12      -0.0879036000
_diffrn_orient_matrix_UB_13      0.0031743000
_diffrn_orient_matrix_UB_21      -0.1230848000
_diffrn_orient_matrix_UB_22      0.0371709000
_diffrn_orient_matrix_UB_23      -0.0730597000
_diffrn_orient_matrix_UB_31      0.0201350000
_diffrn_orient_matrix_UB_32      -0.0311434000
_diffrn_orient_matrix_UB_33      -0.0961868000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0173
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9177
_diffrn_reflns_theta_full        69.8958
_diffrn_reflns_theta_max         69.90
_diffrn_reflns_theta_min         3.96
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.109
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67217
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear whiteish white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.1386
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             876.7482
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.1516
_refine_diff_density_min         -0.2666
_refine_diff_density_rms         0.0418
_refine_ls_d_res_high            0.8209
_refine_ls_d_res_low             11.1512
_refine_ls_goodness_of_fit_ref   1.0269
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    42
_refine_ls_number_parameters     257
_refine_ls_number_reflns         4441
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0269
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0732P)^2^+0.0674P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1235
_refine_ls_wR_factor_ref         0.1400
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -14
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                3138
_reflns_number_total             4441
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1nj00397f2.cif
_cod_data_source_block           L2
_cod_depositor_comments
'Adding full bibliography for 7060433--7060435.cif.'
_cod_database_code               7060433
_chemical_oxdiff_formula         C22H26N4S2ZnI2
_reflns_odcompleteness_completeness 99.28
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. 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
2. Restrained distances
3. Others
 Fixed U11: O1(-8.553428)
4.a Ternary CH refined with riding coordinates:
 C8(H8), C20(H20)
4.b Secondary CH2 refined with riding coordinates:
 C11(H11a,H11b), C12(H12a,H12b)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C18(H18), C6(H6), C5(H5), C4(H4), C17(H17), C16(H16), C15(H15)
4.d Idealised Me refined as rotating group:
 C10(H10a,H10b,H10c), C9(H9a,H9b,H9c), C22(H22a,H22b,H22c), C21(H21a,H21b,H21c)
;
_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 1.670
_oxdiff_exptl_absorpt_empirical_full_min 0.764