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_7060435
_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 Se4, B F4'
_chemical_formula_sum            'C44 H52 B Cu F4 N8 Se4'
_chemical_formula_weight         1159.16
_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             2020-04-06
_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                 91.9405(11)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   33.4425(4)
_cell_length_b                   13.3162(2)
_cell_length_c                   22.4856(3)
_cell_measurement_reflns_used    8505
_cell_measurement_temperature    293
_cell_measurement_theta_max      69.4480
_cell_measurement_theta_min      2.6440
_cell_volume                     10007.7(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      293.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1293
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9206
_diffrn_measured_fraction_theta_max 0.9206
_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     41.00  72.00   1.00    3.67    --    0.00  38.00 150.00   31
  2  \w    -37.00 -12.00   1.00    3.67    --    0.00 113.00-164.00   25
  3  \w    -18.00  26.00   1.00    3.67    --    0.00  38.00 150.00   44
  4  \w     34.00  84.00   1.00   14.71    --   54.00  57.00   0.00   50
  5  \w     33.00  76.00   1.00   14.71    --   54.00 -57.00 -30.00   43
  6  \w     39.00  65.00   1.00   14.71    --   54.00-125.00-180.00   26
  7  \w    -18.00  78.00   1.00   14.71    --   54.00 -38.00  60.00   96
  8  \w     10.00  98.00   1.00   14.71    --   54.00 -99.00-120.00   88
  9  \w     84.00 136.00   1.00   14.71    --  108.00 178.00  60.00   52
 10  \w     81.00 177.00   1.00   14.71    --  108.00  77.00  30.00   96
 11  \w    109.00 135.00   1.00   14.71    --  108.00  50.00  90.00   26
 12  \w     37.00 138.00   1.00   14.71    --  108.00 -77.00-180.00  101
 13  \w     88.00 175.00   1.00   14.71    --  108.00  63.00 -60.00   87
 14  \w    121.00 152.00   1.00   14.71    --  108.00 111.00 -90.00   31
 15  \w     69.00 104.00   1.00   14.71    --  108.00 -63.00 -60.00   35
 16  \w     59.00 143.00   1.00   14.71    --  108.00 178.00-150.00   84
;
_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      -0.0392915000
_diffrn_orient_matrix_UB_12      -0.0500107000
_diffrn_orient_matrix_UB_13      -0.0220956000
_diffrn_orient_matrix_UB_21      0.0227826000
_diffrn_orient_matrix_UB_22      -0.0983357000
_diffrn_orient_matrix_UB_23      -0.0113657000
_diffrn_orient_matrix_UB_31      -0.0078752000
_diffrn_orient_matrix_UB_32      -0.0347948000
_diffrn_orient_matrix_UB_33      0.0638880000
_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  0.0274
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18435
_diffrn_reflns_theta_full        73.4972
_diffrn_reflns_theta_max         73.50
_diffrn_reflns_theta_min         2.64
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.387
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62734
_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    1.5386
_exptl_crystal_description       plate
_exptl_crystal_F_000             4593.3362
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.6140
_refine_diff_density_min         -0.5930
_refine_diff_density_rms         0.0867
_refine_ls_d_res_high            0.8040
_refine_ls_d_res_low             16.7117
_refine_ls_goodness_of_fit_ref   1.0112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    84
_refine_ls_number_parameters     567
_refine_ls_number_reflns         9293
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0112
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0833P)^2^+10.7535P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1216
_refine_ls_wR_factor_ref         0.1413
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              40
_reflns_limit_h_min              -40
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                7261
_reflns_number_total             9293
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1nj00397f2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7060433--7060435.cif.'
_cod_database_code               7060435
_chemical_oxdiff_formula         'C44H52CuN8Se4B F4'
_reflns_odcompleteness_completeness 99.56
_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:
 C42(H42), C31(H31), C22(H22), C11(H11)
2.b Secondary CH2 refined with riding coordinates:
 C35(H35a,H35b), C34(H34a,H34b), C14(H14a,H14b), C15(H15a,H15b)
2.c Aromatic/amide H refined with riding coordinates:
 C37(H37), C40(H40), C38(H38), C17(H17), C18(H18), C6(H6), C7(H7), C20(H20),
 C19(H19), C26(H26), C29(H29), C39(H39), C9(H9), C8(H8), C27(H27), C28(H28)
2.d Idealised Me refined as rotating group:
 C32(H32a,H32b,H32c), C33(H33a,H33b,H33c), C23(H23a,H23b,H23c), C24(H24a,H24b,
 H24c), C12(H12a,H12b,H12c), C44(H44a,H44b,H44c), C13(H13a,H13b,H13c), 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 3.670
_oxdiff_exptl_absorpt_empirical_full_min 0.625