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_7060329
_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         'C32 H36 Hg O4 P2 S4'
_chemical_formula_sum            'C32 H36 Hg O4 P2 S4'
_chemical_formula_weight         875.38
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-18
_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                90
_cell_angle_beta                 106.821(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6282(4)
_cell_length_b                   11.2271(2)
_cell_length_c                   22.4201(7)
_cell_measurement_reflns_used    19621
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      27.3840
_cell_measurement_theta_min      3.2590
_cell_volume                     3524.56(17)
_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      130(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.958
_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    -49.00  -4.00   0.50   12.00    --   -9.95 114.00 124.00   90
  2  \w     -1.00  46.00   0.50   12.00    --   10.22-114.00  33.00   94
  3  \w    -37.00 -11.00   0.50   12.00    --   -9.95 -38.00-150.00   52
  4  \w    -53.00 -22.00   0.50   12.00    --   -9.95 125.00  90.00   62
  5  \w    -18.00  53.00   0.50   12.00    --   -9.95  38.00 150.00  142
  6  \w      5.00  59.00   0.50   12.00    --   10.22-125.00 120.00  108
  7  \w    -15.00  27.00   0.50   12.00    --   10.22  77.00  30.00   84
  8  \w     31.00  63.00   0.50   12.00    --   10.22  77.00  30.00   64
  9  \w    -10.00  43.00   0.50   12.00    --   10.22 -99.00 -30.00  106
 10  \w    -16.00  42.00   0.50   12.00    --   10.22 -99.00-120.00  116
 11  \w     12.00  55.00   0.50   12.00    --   10.22-125.00 -60.00   86
 12  \w    -11.00  14.00   0.50   12.00    --   10.22  77.00  60.00   50
 13  \w     40.00  65.00   0.50   12.00    --   10.22  77.00  60.00   50
 14  \w    -49.00  -5.00   0.50   12.00    --   10.22   0.00 -60.00   88
 15  \w     10.00  58.00   0.50   12.00    --   10.22   0.00 -60.00   96
 16  \w    -50.00 -13.00   0.50   12.00    --   10.22 -38.00-180.00   74
 17  \w    -43.00  -9.00   0.50   12.00    --   10.22 134.00 115.69   68
 18  \w    -53.00  22.00   0.50   12.00    --   10.22 -19.00-120.00  150
;
_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      -0.0502240000
_diffrn_orient_matrix_UB_12      -0.0007623000
_diffrn_orient_matrix_UB_13      -0.0053874000
_diffrn_orient_matrix_UB_21      -0.0063748000
_diffrn_orient_matrix_UB_22      -0.0106716000
_diffrn_orient_matrix_UB_23      -0.0321301000
_diffrn_orient_matrix_UB_31      0.0016918000
_diffrn_orient_matrix_UB_32      -0.0622640000
_diffrn_orient_matrix_UB_33      0.0055853000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            51266
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.420
_diffrn_reflns_theta_min         3.258
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.729
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22031
_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_density_diffrn    1.650
_exptl_crystal_F_000             1736
_refine_diff_density_max         1.055
_refine_diff_density_min         -1.105
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         7697
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0389
_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^)+(0.0200P)^2^+3.9821P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0645
_refine_ls_wR_factor_ref         0.0707
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5394
_reflns_number_total             7697
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj05709f2.cif
_cod_data_source_block           sub-gjp-hg12
_cod_depositor_comments
'Adding full bibliography for 7060328--7060329.cif.'
_cod_database_code               7060329
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Hg P O S C H'
_diffrn_oxdiff_ac3_digest_frames
;
01046486bfc1b9792aa62a0b4a2fa2b2a5000250399
;
_diffrn_oxdiff_ac3_digest_hkl
;
01567bfa1fcf002cc7128d36e6e1da7d8e277e
;
_reflns_odcompleteness_completeness 99.75
_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:
 C26(H26), C18(H18), C30(H30), C3(H3), C2(H2), C29(H29), C6(H6), C11(H11),
 C10(H10), C14(H14), C22(H22), C21(H21)
2.b Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C31(H31A,H31B,H31C), C7(H7A,H7B,H7C), C15(H15A,H15B,
 H15C), C24(H24A,H24B,H24C), C8(H8A,H8B,H8C), C16(H16A,H16B,H16C), C23(H23A,
 H23B,H23C)
;
_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 2.993
_oxdiff_exptl_absorpt_empirical_full_min 0.554