Role of non-covalent interactions in the supramolecular architectures of mercury(ii) diphenyldithiophosphates: An experimental and theoretical investigation
Kumar, Pretam; Banerjee, Snehasis; Radha, Anu; Firdoos, Tahira; Sahoo, Subash Chandra; Pandey, Sushil K.; New Journal of Chemistry 45 (2021) 2249–2263; doi:10.1039/D0NJ05709F

data_7060328
_publ_section_title
;
 Role of non-covalent interactions in the supramolecular architectures of
 mercury(ii) diphenyldithiophosphates: An experimental and theoretical
 investigation
;
_journal_issue                   4
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2249
_journal_page_last               2263
_journal_paper_doi               10.1039/D0NJ05709F
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C40 H52 Hg O4 P2 S4'
_chemical_formula_sum            'C40 H52 Hg O4 P2 S4'
_chemical_formula_weight         987.58
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-07-25
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.01.05 svn.r3372 for Rigaku Oxford Diffraction, GUI svn.r5289)
;
_audit_update_record
;
2020-08-31 deposited with the CCDC.	2020-12-29 downloaded from the CCDC.
;
_cell_angle_alpha                81.444(2)
_cell_angle_beta                 85.958(2)
_cell_angle_gamma                87.659(2)
_cell_formula_units_Z            2
_cell_length_a                   10.2272(2)
_cell_length_b                   12.2502(2)
_cell_length_c                   17.0456(3)
_cell_measurement_reflns_used    20015
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4100
_cell_measurement_theta_min      3.4990
_cell_volume                     2105.54(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.973
_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    -74.00 -28.00   0.50    5.00    --   -9.95 154.00-134.00   92
  2  \w    -52.00 -27.00   0.50    5.00    --   -9.95 121.00  67.00   50
  3  \w      4.00  29.00   0.50    5.00    --   10.22-121.00 -15.00   50
  4  \w     37.00  75.00   0.50    5.00    --   10.22-154.00-173.00   76
  5  \w    -58.00 -24.00   0.50    5.00    --   -9.95 125.00-180.00   68
  6  \w    -74.00   4.00   0.50    5.00    --   -9.95 -38.00-120.00  156
  7  \w    -23.00  35.00   0.50    5.00    --   -9.95  38.00  90.00  116
  8  \w    -58.00 -15.00   0.50    5.00    --   -9.95 125.00  30.00   86
  9  \w    -58.00 -23.00   0.50    5.00    --   -9.95 125.00 120.00   70
 10  \w      0.00  26.00   0.50    5.00    --   10.22  38.00-180.00   52
 11  \w    -38.00  -7.00   0.50    5.00    --   10.22 132.00-129.15   62
 12  \w    -33.00  -4.00   0.50    5.00    --   10.22 125.00  49.56   58
 13  \w    -11.00  43.00   0.50    5.00    --   10.22 -99.00 -90.00  108
 14  \w    -22.00   7.00   0.50    5.00    --   10.22 -19.00 -30.00   58
 15  \w    -58.00 -32.00   0.50    5.00    --   10.22 -19.00 -30.00   52
 16  \w    -19.00  42.00   0.50    5.00    --   10.22 -99.00  30.00  122
 17  \w    -55.00   7.50   0.50    5.00    --   10.22 -19.00  90.00  125
;
_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      -0.0239850000
_diffrn_orient_matrix_UB_12      -0.0026073000
_diffrn_orient_matrix_UB_13      -0.0376992000
_diffrn_orient_matrix_UB_21      0.0636940000
_diffrn_orient_matrix_UB_22      0.0100528000
_diffrn_orient_matrix_UB_23      -0.0182790000
_diffrn_orient_matrix_UB_31      0.0143659000
_diffrn_orient_matrix_UB_32      -0.0576527000
_diffrn_orient_matrix_UB_33      0.0047899000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0668
_diffrn_reflns_av_unetI/netI     0.0600
_diffrn_reflns_Laue_measured_fraction_full 0.950
_diffrn_reflns_Laue_measured_fraction_max 0.880
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27664
_diffrn_reflns_point_group_measured_fraction_full 0.950
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.470
_diffrn_reflns_theta_min         3.239
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.968
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47117
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_description       block
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.996
_refine_diff_density_min         -2.326
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         8474
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0357
_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^)+(0.0324P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0781
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7437
_reflns_number_total             8474
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj05709f2.cif
_cod_data_source_block           sub-iitm
_cod_depositor_comments
'Adding full bibliography for 7060328--7060329.cif.'
_cod_original_cell_volume        2105.55(7)
_cod_database_code               7060328
_publcif_datablock.id            {2c53e1cd-1ce1-4e91-8346-e274fd5a7f7f}
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Hg P S C H N O'
_diffrn_oxdiff_ac3_digest_frames
;
018c8dd51d651682759a106ff5c8ffa40300025e04d
;
_diffrn_oxdiff_ac3_digest_hkl
;
01bc9c1ba5542e553efd2d4ad621315863e842
;
_reflns_odcompleteness_completeness 94.16
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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:
 C22(H22), C23(H23), C25(H25), C36(H36), C16(H16), C26(H26), C3(H3), C2(H2),
 C35(H35), C12(H12), C13(H13), C15(H15), C32(H32), C33(H33), C5(H5), C6(H6)
2.b Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C20(H20A,H20B,H20C), C19(H19A,H19B,H19C), C8(H8A,H8B,
 H8C), C40(H40A,H40B,H40C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C39(H39A,H39B,
 H39C), C18(H18A,H18B,H18C), C30(H30A,H30B,H30C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C)
;
_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 1.407
_oxdiff_exptl_absorpt_empirical_full_min 0.634