2-Pyrrolylthiones as Monoanionic Bidentate N,S-Chelators: Synthesis and Molecular Structure of 2-Pyrrolylthionato Complexes of Nickel(II), Cobalt(III), and Mercury(II)
Christian Brückner; Stephen J. Rettig; David Dolphin; Inorganic Chemistry 39 (2000) 6100–6106; doi:10.1021/ic0004636

data_4321682
_publ_contact_author_address
;
Department of Chemistry, U-60
University of Connecticut
55 N. Eagleville Rd.
Storrs,  CT 06269-3060
;
_publ_contact_author_email       bruckner@nucleus.chem.uconn.edu
_publ_contact_author_fax         860-486-2981
_publ_contact_author_name        'Christian Br\"uckner'
_publ_contact_author_phone       860-486-2743
_publ_section_title
;
 2-Pyrrolylthiones as Monoanionic Bidentate N,S-Chelators: Synthesis and
 Molecular Structure of 2-Pyrrolylthionato Complexes of Nickel(II),
 Cobalt(III), and Mercury(II)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6100
_journal_page_last               6106
_journal_paper_doi               10.1021/ic0004636
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C18 H14.57 N4 Ni O0.28 S2'
_chemical_formula_weight         414.25
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_audit_creation_method           'teXsan v1.8'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   18.4666(11)
_cell_length_b                   18.4666(11)
_cell_length_c                   26.404(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294.2
_cell_measurement_theta_max      37.8
_cell_measurement_theta_min      28.8
_cell_volume                     7797.8(9)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1992-1997)'
_computing_publication_material  'teXsan (MSC, 1992-1997)'
_computing_structure_refinement  'teXsan (MSC, 1992-1997)'
_computing_structure_solution
;
SIR88 (Burla, et. al. 1989)
;
_diffrn_ambient_temperature      294.2
_diffrn_measurement_device_type  'Rigaku AFC6S'
_diffrn_orient_matrix_UB_11      -0.05449
_diffrn_orient_matrix_UB_12      -0.03694
_diffrn_orient_matrix_UB_13      -0.01730
_diffrn_orient_matrix_UB_21      0.01250
_diffrn_orient_matrix_UB_22      -0.04681
_diffrn_orient_matrix_UB_23      0.00010
_diffrn_orient_matrix_UB_31      -0.02801
_diffrn_orient_matrix_UB_32      -0.01882
_diffrn_orient_matrix_UB_33      0.03369
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.03743
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            3912
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         77.66
_diffrn_reflns_theta_min         3.23
_diffrn_standards_decay_%        -1.04
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.947
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.770
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             3830.94
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.56
_refine_diff_density_min         -0.23
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.780
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    2
_refine_ls_number_parameters     230
_refine_ls_number_reflns         2234
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo)]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_ref         0.0330
_reflns_number_gt                2234
_reflns_number_total             3665
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            ic0004636_2.cif
_cod_data_source_block           compound_14
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        7797.9(10)
_cod_original_sg_symbol_H-M      'R -3 '
_cod_original_formula_sum        'C18 H14.57 N4 O0.28 Ni S2 '
_cod_database_code               4321682