A Structural Study of Dithizone Coordination Chemistry
Rice, Craig; Jewsbury, R. A.; Dunmore, Rachel Ellen; Bullock, Samantha; Faulkner, Robert Allan; CrystEngComm  (2017) –; doi:10.1039/C7CE00580F

data_7228369
_publ_section_title
;
 A Structural Study of Dithizone Coordination Chemistry
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE00580F
_journal_year                    2017
_chemical_formula_moiety         'C26 H22 Hg N8 S2, 2(C2 H3 N)'
_chemical_formula_sum            'C30 H28 Hg N10 O0 S2'
_chemical_formula_weight         793.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-06-20 deposited with the CCDC.
2017-06-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.577(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.7448(19)
_cell_length_b                   5.3260(4)
_cell_length_c                   13.8216(11)
_cell_measurement_reflns_used    6638
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.98
_cell_measurement_theta_min      2.47
_cell_volume                     1534.2(2)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0817
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7784
_diffrn_reflns_point_group_measured_fraction_full 0.907
_diffrn_reflns_point_group_measured_fraction_max 0.865
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.418
_diffrn_reflns_theta_min         1.537
_exptl_absorpt_coefficient_mu    5.191
_exptl_absorpt_correction_T_max  0.9499
_exptl_absorpt_correction_T_min  0.6248
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_description       needle
_exptl_crystal_F_000             780
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.683
_refine_diff_density_min         -0.777
_refine_diff_density_rms         0.121
_refine_ls_abs_structure_details
;
 Flack x determined using 1072 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.024(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.815
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         3329
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.815
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0542
_refine_ls_wR_factor_ref         0.0553
_reflns_Friedel_coverage         0.578
_reflns_Friedel_fraction_full    0.791
_reflns_Friedel_fraction_max     0.708
_reflns_number_gt                3240
_reflns_number_total             3329
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00580f2.cif
_cod_data_source_block           mo_Rachel_AgHg_0m
_cod_database_code               7228369
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.625
_shelx_estimated_absorpt_t_max   0.950
_shelx_res_checksum              99855