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_7057549
_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         'C46 H38 Hg N6 O4, 2(F6 P), 0.75(C2 H3 N)'
_chemical_formula_sum            'C47.5 H40.25 F12 Hg N6.75 O4 P2'
_chemical_formula_weight         1260.14
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                79.7510(10)
_cell_angle_beta                 76.1130(10)
_cell_angle_gamma                68.3030(10)
_cell_formula_units_Z            2
_cell_length_a                   13.5575(10)
_cell_length_b                   13.6764(10)
_cell_length_c                   15.6816(12)
_cell_measurement_reflns_used    3708
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.18
_cell_measurement_theta_min      2.20
_cell_volume                     2609.8(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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      296.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0292
_diffrn_reflns_av_unetI/netI     0.0629
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13495
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         1.344
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.101
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6324
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1264 before and 0.0347 after correction. The Ratio of minimum to maximum transmission is 0.8481. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1245
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.046
_refine_diff_density_min         -1.007
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     696
_refine_ls_number_reflns         9154
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0491
_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^)+(0.0808P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1248
_refine_ls_wR_factor_ref         0.1372
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7193
_reflns_number_total             9154
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj02029a2.cif
_cod_data_source_block           n120929b
_cod_depositor_comments
'Adding full bibliography for 7057549--7057551.cif.'
_cod_original_formula_sum        'C47.50 H40.25 F12 Hg N6.75 O4 P2'
_cod_database_code               7057549
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.671
_shelx_estimated_absorpt_t_min   0.621
_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
 N8-C50 = N7-C48
 2.7 with sigma of 0.01
 N8-C49 = N7-C47
 1.2 with sigma of 0.005
 C49-C50 = C47-C48
 1.48 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C49) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C48)
\\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(N8) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: C47(0.5) N7(0.5) C48(0.5) H48A(0.5) H48B(0.5) H48C(0.5) C49(0.25)
 C50(0.25) H50A(0.25) H50B(0.25) H50C(0.25) N8(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C32(H32A,H32B),
 C33(H33A,H33B), C31(H31A,H31B), C41(H41A,H41B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12), C13(H13),
 C18(H18), C19(H19), C20(H20), C28(H28), C29(H29), C30(H30), C37(H37), C38(H38),
  C39(H39), C40(H40), C43(H43), C44(H44), C45(H45), C46(H46)
5.c Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C), C50(H50A,H50B,H50C)
;
_olex2_submission_special_instructions 'No special instructions were received'