#------------------------------------------------------------------------------
#$Date: 2020-08-06 16:02:15 +0200 (jue 06 de ago de 2020) $
#$Revision: 254985 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/46/7704628.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7704628
loop_
_publ_author_name
'Raju, Saravanan'
'Singh, Harkesh B.'
'Butcher, Ray J.'
_publ_section_title
;
 Metallophilic interactions: observations of the shortest
 metallophilicinteractions between closed shell
 (d¹⁰d¹⁰, d¹⁰d⁸,
 d⁸d⁸) metal ions [MM' M = Hg(ii) and Pd(ii) and M'
 = Cu(i), Ag(i), Au(i), and Pd(ii)].
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9099
_journal_page_last               9117
_journal_paper_doi               10.1039/d0dt01008a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C20 H14 Hg'
_chemical_formula_sum            'C20 H14 Hg'
_chemical_formula_weight         454.90
_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
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2020-02-17 deposited with the CCDC.	2020-06-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.263(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.78920(10)
_cell_length_b                   11.4477(3)
_cell_length_c                   25.3709(6)
_cell_measurement_reflns_used    11046
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.2470
_cell_measurement_theta_min      2.3880
_cell_volume                     1390.95(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Shelxtl (Sheldrick, 2008)'
_computing_publication_material  'Shelxtl (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'Shelxt (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            19566
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.217
_diffrn_reflns_theta_min         1.779
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    11.054
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear intense colourless'
_exptl_crystal_density_diffrn    2.172
_exptl_crystal_description       needle
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.038
_refine_diff_density_max         3.942
_refine_diff_density_min         -0.961
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         4194
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0297
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0384P)²+4.2749P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0762
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3604
_reflns_number_total             4194
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt01008a2.cif
_cod_data_source_block           Ligand_1
_cod_depositor_comments
'Adding full bibliography for 7704622--7704632.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7704628
_shelx_shelxl_version_number     2018/1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Hg Hg 0.57580(3) 0.41735(2) 0.63057(2) 0.02005(6) Uani 1 1 d . . . . .
C1 C 0.4129(9) 0.5809(3) 0.64722(17) 0.0200(8) Uani 1 1 d . . . . .
C2 C 0.2041(9) 0.6337(4) 0.61795(16) 0.0214(8) Uani 1 1 d . . . . .
H2A H 0.111771 0.590435 0.591081 0.026 Uiso 1 1 calc R U . . .
C3 C 0.1258(9) 0.7502(4) 0.62725(16) 0.0243(8) Uani 1 1 d . . . . .
H3A H -0.017060 0.784594 0.606297 0.029 Uiso 1 1 calc R U . . .
C4 C 0.2523(9) 0.8152(3) 0.66609(17) 0.0222(8) Uani 1 1 d . . . . .
H4A H 0.197394 0.893848 0.671853 0.027 Uiso 1 1 calc R U . . .
C5 C 0.4646(8) 0.7644(4) 0.69743(16) 0.0214(8) Uani 1 1 d . . . . .
C6 C 0.6045(10) 0.8266(4) 0.73794(18) 0.0265(9) Uani 1 1 d . . . . .
H6A H 0.557784 0.905649 0.745064 0.032 Uiso 1 1 calc R U . . .
C7 C 0.8081(10) 0.7714(4) 0.76674(18) 0.0288(9) Uani 1 1 d . . . . .
H7A H 0.905730 0.811299 0.793986 0.035 Uiso 1 1 calc R U . . .
C8 C 0.8692(10) 0.6530(4) 0.75478(18) 0.0286(9) Uani 1 1 d . . . . .
H8A H 1.010784 0.615186 0.774837 0.034 Uiso 1 1 calc R U . . .
C9 C 0.7440(8) 0.5929(3) 0.71815(15) 0.0178(7) Uani 1 1 d . . . . .
H9A H 0.791834 0.513432 0.712234 0.021 Uiso 1 1 calc R U . . .
C10 C 0.5420(8) 0.6460(4) 0.68828(16) 0.0202(8) Uani 1 1 d . . . . .
C11 C 0.7500(9) 0.2581(4) 0.60958(16) 0.0217(7) Uani 1 1 d . . . . .
C12 C 0.6759(9) 0.1506(4) 0.63006(17) 0.0234(8) Uani 1 1 d . . . . .
H12A H 0.539440 0.146808 0.657062 0.028 Uiso 1 1 calc R U . . .
C13 C 0.7994(10) 0.0460(4) 0.61157(18) 0.0258(9) Uani 1 1 d . . . . .
H13A H 0.742235 -0.026747 0.625937 0.031 Uiso 1 1 calc R U . . .
C14 C 0.9984(9) 0.0482(4) 0.57363(18) 0.0252(9) Uani 1 1 d . . . . .
H14A H 1.081872 -0.022495 0.561994 0.030 Uiso 1 1 calc R U . . .
C15 C 1.0812(8) 0.1568(4) 0.55140(16) 0.0199(7) Uani 1 1 d . . . . .
C16 C 1.2852(9) 0.1659(4) 0.51092(17) 0.0253(9) Uani 1 1 d . . . . .
H16A H 1.376104 0.098044 0.497995 0.030 Uiso 1 1 calc R U . . .
C17 C 1.3486(10) 0.2734(4) 0.49089(18) 0.0277(9) Uani 1 1 d . . . . .
H17A H 1.484137 0.281484 0.463904 0.033 Uiso 1 1 calc R U . . .
C18 C 1.2104(9) 0.3715(4) 0.51086(18) 0.0259(9) Uani 1 1 d . . . . .
H18A H 1.254379 0.445636 0.496241 0.031 Uiso 1 1 calc R U . . .
C19 C 1.0224(8) 0.3675(3) 0.54880(14) 0.0145(6) Uani 1 1 d . . . . .
H19A H 0.935803 0.436706 0.561313 0.017 Uiso 1 1 calc R U . . .
C20 C 0.9563(8) 0.2612(3) 0.56946(15) 0.0188(7) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Hg C11 176.35(16) . . ?
C2 C1 C10 118.5(4) . . ?
C2 C1 Hg 123.9(3) . . ?
C10 C1 Hg 117.4(3) . . ?
C1 C2 C3 121.2(4) . . ?
C1 C2 H2A 119.4 . . ?
C3 C2 H2A 119.4 . . ?
C4 C3 C2 121.1(4) . . ?
C4 C3 H3A 119.4 . . ?
C2 C3 H3A 119.4 . . ?
C3 C4 C5 119.7(4) . . ?
C3 C4 H4A 120.2 . . ?
C5 C4 H4A 120.2 . . ?
C4 C5 C6 122.6(4) . . ?
C4 C5 C10 119.1(4) . . ?
C6 C5 C10 118.3(4) . . ?
C7 C6 C5 119.2(4) . . ?
C7 C6 H6A 120.4 . . ?
C5 C6 H6A 120.4 . . ?
C6 C7 C8 118.2(4) . . ?
C6 C7 H7A 120.9 . . ?
C8 C7 H7A 120.9 . . ?
C9 C8 C7 124.2(4) . . ?
C9 C8 H8A 117.9 . . ?
C7 C8 H8A 117.9 . . ?
C8 C9 C10 118.9(4) . . ?
C8 C9 H9A 120.6 . . ?
C10 C9 H9A 120.6 . . ?
C9 C10 C1 118.5(4) . . ?
C9 C10 C5 121.1(4) . . ?
C1 C10 C5 120.4(4) . . ?
C12 C11 C20 118.1(4) . . ?
C12 C11 Hg 125.5(3) . . ?
C20 C11 Hg 116.3(3) . . ?
C11 C12 C13 121.3(4) . . ?
C11 C12 H12A 119.3 . . ?
C13 C12 H12A 119.3 . . ?
C14 C13 C12 121.0(4) . . ?
C14 C13 H13A 119.5 . . ?
C12 C13 H13A 119.5 . . ?
C13 C14 C15 119.7(4) . . ?
C13 C14 H14A 120.2 . . ?
C15 C14 H14A 120.2 . . ?
C20 C15 C14 119.4(4) . . ?
C20 C15 C16 117.7(4) . . ?
C14 C15 C16 122.9(4) . . ?
C17 C16 C15 119.3(4) . . ?
C17 C16 H16A 120.4 . . ?
C15 C16 H16A 120.4 . . ?
C16 C17 C18 118.8(4) . . ?
C16 C17 H17A 120.6 . . ?
C18 C17 H17A 120.6 . . ?
C19 C18 C17 124.1(4) . . ?
C19 C18 H18A 118.0 . . ?
C17 C18 H18A 118.0 . . ?
C18 C19 C20 118.2(4) . . ?
C18 C19 H19A 120.9 . . ?
C20 C19 H19A 120.9 . . ?
C19 C20 C15 122.0(4) . . ?
C19 C20 C11 117.5(4) . . ?
C15 C20 C11 120.5(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Hg C1 2.073(4) . ?
Hg C11 2.076(4) . ?
C1 C2 1.382(6) . ?
C1 C10 1.420(6) . ?
C2 C3 1.406(6) . ?
C2 H2A 0.9500 . ?
C3 C4 1.373(6) . ?
C3 H3A 0.9500 . ?
C4 C5 1.413(6) . ?
C4 H4A 0.9500 . ?
C5 C6 1.416(6) . ?
C5 C10 1.424(6) . ?
C6 C7 1.370(7) . ?
C6 H6A 0.9500 . ?
C7 C8 1.420(7) . ?
C7 H7A 0.9500 . ?
C8 C9 1.301(6) . ?
C8 H8A 0.9500 . ?
C9 C10 1.369(6) . ?
C9 H9A 0.9500 . ?
C11 C12 1.382(6) . ?
C11 C20 1.422(6) . ?
C12 C13 1.416(6) . ?
C12 H12A 0.9500 . ?
C13 C14 1.358(7) . ?
C13 H13A 0.9500 . ?
C14 C15 1.422(6) . ?
C14 H14A 0.9500 . ?
C15 C20 1.414(5) . ?
C15 C16 1.425(6) . ?
C16 C17 1.366(6) . ?
C16 H16A 0.9500 . ?
C17 C18 1.400(6) . ?
C17 H17A 0.9500 . ?
C18 C19 1.322(6) . ?
C18 H18A 0.9500 . ?
C19 C20 1.363(5) . ?
C19 H19A 0.9500 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C10 C1 C2 C3 1.9(6) . . . . ?
Hg C1 C2 C3 -172.2(3) . . . . ?
C1 C2 C3 C4 -0.7(6) . . . . ?
C2 C3 C4 C5 -0.1(6) . . . . ?
C3 C4 C5 C6 179.7(4) . . . . ?
C3 C4 C5 C10 -0.4(6) . . . . ?
C4 C5 C6 C7 179.9(4) . . . . ?
C10 C5 C6 C7 0.0(6) . . . . ?
C5 C6 C7 C8 -0.4(6) . . . . ?
C6 C7 C8 C9 -0.1(7) . . . . ?
C7 C8 C9 C10 0.9(7) . . . . ?
C8 C9 C10 C1 177.9(4) . . . . ?
C8 C9 C10 C5 -1.2(6) . . . . ?
C2 C1 C10 C9 178.4(4) . . . . ?
Hg C1 C10 C9 -7.1(5) . . . . ?
C2 C1 C10 C5 -2.5(6) . . . . ?
Hg C1 C10 C5 172.0(3) . . . . ?
C4 C5 C10 C9 -179.1(4) . . . . ?
C6 C5 C10 C9 0.8(6) . . . . ?
C4 C5 C10 C1 1.7(6) . . . . ?
C6 C5 C10 C1 -178.4(4) . . . . ?
C20 C11 C12 C13 -0.4(6) . . . . ?
Hg C11 C12 C13 177.4(3) . . . . ?
C11 C12 C13 C14 1.1(7) . . . . ?
C12 C13 C14 C15 -1.1(7) . . . . ?
C13 C14 C15 C20 0.5(6) . . . . ?
C13 C14 C15 C16 -179.0(4) . . . . ?
C20 C15 C16 C17 -0.9(6) . . . . ?
C14 C15 C16 C17 178.6(4) . . . . ?
C15 C16 C17 C18 0.0(7) . . . . ?
C16 C17 C18 C19 0.9(7) . . . . ?
C17 C18 C19 C20 -0.8(6) . . . . ?
C18 C19 C20 C15 -0.3(6) . . . . ?
C18 C19 C20 C11 -178.9(4) . . . . ?
C14 C15 C20 C19 -178.4(4) . . . . ?
C16 C15 C20 C19 1.1(6) . . . . ?
C14 C15 C20 C11 0.1(6) . . . . ?
C16 C15 C20 C11 179.6(4) . . . . ?
C12 C11 C20 C19 178.5(4) . . . . ?
Hg C11 C20 C19 0.5(5) . . . . ?
C12 C11 C20 C15 -0.1(6) . . . . ?
Hg C11 C20 C15 -178.2(3) . . . . ?
