NHC Hg(ii) and Pd(ii) complexes based on 1,8-dihydroxy-9,10-anthraquinone: synthesis, structure and catalysis
Zhao, Zhi-Xiang; Hu, Ze-Liang; Yu, Shao-Cong; Liu, Qing-Xiang; New Journal of Chemistry 42 (2018) 13329–; doi:10.1039/C8NJ02029A

data_7057550
_publ_section_title
;
 NHC Hg(ii) and Pd(ii) complexes based on
 1,8-dihydroxy-9,10-anthraquinone: synthesis, structure and catalysis
;
_journal_issue                   16
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              13329
_journal_paper_doi               10.1039/C8NJ02029A
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C34 H36 Br2 Hg N6 O3'
_chemical_formula_sum            'C34 H36 Br2 Hg N6 O3'
_chemical_formula_weight         937.10
_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_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-06-11
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-06-26 deposited with the CCDC.
2018-07-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.258(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.398(2)
_cell_length_b                   21.286(3)
_cell_length_c                   12.4804(16)
_cell_measurement_reflns_used    5194
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.99
_cell_measurement_theta_min      2.60
_cell_volume                     3785.8(9)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9476
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.008
_diffrn_reflns_theta_max         25.008
_diffrn_reflns_theta_min         1.720
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.216
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3096
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1293 before and 0.0522 after correction. The Ratio of minimum to maximum transmission is 0.4152. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_description       block
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_platon_squeeze_details
;
TITL N120606A  C 2/c        R = 0.05
CELL   15.3980   21.2860   12.4804     90.00    112.26     90.00
SPGR C2/c
C101 0.500 0.281 0.243 !       6.52 eA-3
C102 0.433 0.312 0.172 !       4.25 eA-3
C103 0.358 0.282 0.082 !       3.72 eA-3
Q104 0.956 0.454 0.233 !       2.73 eA-3
C105 0.360 0.324 0.141 !       2.06 eA-3
Q106 0.042 0.394 0.271 !       1.99 eA-3
Q107 0.827 0.373 0.299 !       1.39 eA-3
Q108 0.923 0.313 0.309 !       1.02 eA-3
Q109 0.015 0.419 0.310 !       1.00 eA-3
Q110 0.158 0.313 0.196 !       0.82 eA-3
C111 0.357 0.269 0.008 !       0.75 eA-3
Q112 0.927 0.375 0.326 !       0.72 eA-3
C113 0.713 0.260 0.483 !       0.70 eA-3
Q114 0.047 0.345 0.141 !       0.69 eA-3
C115 0.467 0.346 0.121 !       0.64 eA-3
Q116 0.045 0.207 0.436 !       0.59 eA-3
Q117 0.063 0.424 0.365 !       0.57 eA-3
C118 0.536 0.320 0.401 !       0.55 eA-3
Q119 0.108 0.174 0.263 !       0.54 eA-3
Q120 0.672 0.125 0.024 !       0.50 eA-3
;
_refine_diff_density_max         2.639
_refine_diff_density_min         -2.462
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         3343
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0336
_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^)+(0.0572P)^2^+0.9261P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.0891
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2984
_reflns_number_total             3343
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj02029a2.cif
_cod_data_source_block           n120606a_sq
_cod_depositor_comments
'Adding full bibliography for 7057549--7057551.cif.'
_cod_database_code               7057550
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.436
_shelx_estimated_absorpt_t_min   0.401
_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. Restrained distances
 C15A-C11 = C15-C11
 1.5 with sigma of 0.01
 O2A-C15A = O2-C15
 1.24 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C15) = Uanis(C15A)
Uanis(O2) = Uanis(O2A)
4. Others
 Sof(O2A)=Sof(C15A)=0.5*(1-FVAR(2))
 Sof(O2)=Sof(C15)=0.5*FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C2(H2a,H2b), C6(H6a,H6b), C7(H7a,H7b), C8(H8a,H8b), C17(H17a,H17b)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C12(H12), C13(H13), C14(H14)
5.c Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'