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_7057551
_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         'C47 H44 Hg N4 O8, 2(F6 P)'
_chemical_formula_sum            'C47 H44 F12 Hg N4 O8 P2'
_chemical_formula_weight         1283.39
_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                 100.675(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.023(4)
_cell_length_b                   12.719(3)
_cell_length_c                   18.421(5)
_cell_measurement_reflns_used    3005
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.38
_cell_measurement_theta_min      2.28
_cell_volume                     4840(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0656
_diffrn_reflns_av_unetI/netI     0.0681
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12096
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.008
_diffrn_reflns_theta_max         25.008
_diffrn_reflns_theta_min         1.880
_exptl_absorpt_coefficient_mu    3.351
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5371
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1275 before and 0.0407 after correction. The Ratio of minimum to maximum transmission is 0.7203. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2544
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.463
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.128
_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     336
_refine_ls_number_reflns         4249
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0414
_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/[\s^2^(Fo^2^)+(0.0435P)^2^+3.0181P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.0930
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3670
_reflns_number_total             4249
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj02029a2.cif
_cod_data_source_block           n121019a
_cod_depositor_comments
'Adding full bibliography for 7057549--7057551.cif.'
_cod_database_code               7057551
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.670
_shelx_estimated_absorpt_t_min   0.633
_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. Uiso/Uaniso restraints and constraints
Uanis(F6) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(C14) \\sim
Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C20) \\sim Ueq,
Uanis(C19) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
Uanis(C24) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C17)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
3. Others
 Fixed Sof: H24A(0.5) H24B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C23(H23A,H23B), C24(H24A,
 H24B)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C14(H14), C15(H15), C16(H16), C20(H20), C21(H21), C22(H22)
4.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_olex2_submission_special_instructions 'No special instructions were received'