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_7060434
_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         'C44 H52 Cu N8 S4, B F4'
_chemical_formula_sum            'C44 H52 B Cu F4 N8 S4'
_chemical_formula_weight         971.58
_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'
_symmetry_Int_Tables_number      15
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-02-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-02-18 deposited with the CCDC.	2021-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.7456(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   33.0313(4)
_cell_length_b                   13.34528(14)
_cell_length_c                   22.2766(2)
_cell_measurement_reflns_used    8197
_cell_measurement_temperature    298
_cell_measurement_theta_max      69.7890
_cell_measurement_theta_min      3.5660
_cell_volume                     9808.52(18)
_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 0.9722
_diffrn_measured_fraction_theta_max 0.9722
_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     32.00  58.00   1.00    3.83    --    0.00  57.00  90.00   26
  2  \w    -22.00  22.00   1.00    3.83    --    0.00  57.00  90.00   44
  3  \w     -3.00  32.00   1.00    3.83    --    0.00  57.00-180.00   35
  4  \w     43.00 122.00   1.00   15.31    --   54.00  57.00  60.00   79
  5  \w     -3.00  70.00   1.00   15.31    --   54.00 -57.00  90.00   73
  6  \w     32.00  58.00   1.00   15.31    --   54.00 -99.00 120.00   26
  7  \w     49.00 112.00   1.00   15.31    --   54.00-125.00 -30.00   63
  8  \w     12.00  74.00   1.00   15.31    --   54.00 -57.00 150.00   62
  9  \w    102.00 178.00   1.00   15.31    --  108.00 111.00 120.00   76
 10  \w     87.00 178.00   1.00   15.31    --  108.00  50.00 -90.00   91
 11  \w     41.00  84.00   1.00   15.31    --  108.00 -63.00 120.00   43
 12  \w    109.00 156.00   1.00   15.31    --  108.00 111.00-180.00   47
 13  \w     58.00 125.00   1.00   15.31    --  108.00 -50.00 120.00   67
 14  \w     67.00 105.00   1.00   15.31    --  108.00-111.00-120.00   38
 15  \w     70.00 136.00   1.00   15.31    --  108.00 -77.00   0.00   66
 16  \w    123.00 149.00   1.00   15.31    --  108.00 178.00  30.00   26
 17  \w     75.00 102.00   1.00   15.31    --  108.00 178.00  30.00   27
;
_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      -0.0145040000
_diffrn_orient_matrix_UB_12      -0.0561215000
_diffrn_orient_matrix_UB_13      0.0555016000
_diffrn_orient_matrix_UB_21      -0.0436699000
_diffrn_orient_matrix_UB_22      0.0005155000
_diffrn_orient_matrix_UB_23      -0.0274588000
_diffrn_orient_matrix_UB_31      0.0078076000
_diffrn_orient_matrix_UB_32      -0.1009420000
_diffrn_orient_matrix_UB_33      -0.0309560000
_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  0.0149
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            17505
_diffrn_reflns_theta_full        69.9154
_diffrn_reflns_theta_max         69.92
_diffrn_reflns_theta_min         2.68
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.672
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79620
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.3158
_exptl_crystal_description       plate
_exptl_crystal_F_000             4053.6175
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.4847
_refine_diff_density_min         -0.6639
_refine_diff_density_rms         0.0662
_refine_ls_d_res_high            0.8208
_refine_ls_d_res_low             16.4967
_refine_ls_goodness_of_fit_ref   1.0500
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    84
_refine_ls_number_parameters     567
_refine_ls_number_reflns         9042
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0500
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0506
_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^)+(0.1012P)^2^+9.5494P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1566
_refine_ls_wR_factor_ref         0.1726
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              39
_reflns_limit_h_min              -39
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                7358
_reflns_number_total             9042
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1nj00397f2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7060433--7060435.cif.'
_cod_original_cell_volume        9808.51(18)
_cod_database_code               7060434
_chemical_oxdiff_formula         C22H26N4S2CuBF4
_reflns_odcompleteness_completeness 99.05
_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.a Ternary CH refined with riding coordinates:
 C5(H5), C22(H22), C25(H25), C42(H42)
2.b Secondary CH2 refined with riding coordinates:
 C15(H15a,H15b), C14(H14a,H14b), C34(H34a,H34b), C35(H35a,H35b)
2.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C18(H18), C20(H20), C19(H19), C12(H12), C11(H11), C9(H9), C32(H32),
 C37(H37), C31(H31), C29(H29), C38(H38), C39(H39), C40(H40), C10(H10), C30(H30)
2.d Idealised Me refined as rotating group:
 C6(H6a,H6b,H6c), C7(H7a,H7b,H7c), C23(H23a,H23b,H23c), C24(H24a,H24b,H24c),
 C27(H27a,H27b,H27c), C44(H44a,H44b,H44c), C26(H26a,H26b,H26c), C43(H43a,H43b,
 H43c)
;
_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 1.570
_oxdiff_exptl_absorpt_empirical_full_min 0.715