Structural dependence of π‒π interactions in dithiocarbazato and thiosemicarbazato nickel complexes
Liu Ze-hua; Duan Chun-ying; Li Ji-hui; Liu Yong-jiang; Mei Yu-hua; You Xiao-zeng; New J. Chem. 24 (2000) 1057–1062; doi:10.1039/b004846l

data_7051352
_publ_section_title
;
 Structural dependence of \p--\p interactions in dithiocarbazato and
 thiosemicarbazato nickel complexes
;
_journal_issue                   12
_journal_name_full               'New J. Chem.'
_journal_page_first              1057
_journal_page_last               1062
_journal_paper_doi               10.1039/b004846l
_journal_volume                  24
_journal_year                    2000
_chemical_formula_sum            'C28 H22 N6 Ni O S2'
_chemical_formula_weight         581.35
_chemical_name_systematic
; 
bis(fluorene-9-one thiosemicarbazato)nickel monohydrate 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                91.439(14)
_cell_angle_beta                 99.301(12)
_cell_angle_gamma                106.954(12)
_cell_formula_units_Z            4
_cell_length_a                   12.2943(14)
_cell_length_b                   14.670(2)
_cell_length_c                   15.508(2)
_cell_measurement_reflns_used    41
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      12.21
_cell_measurement_theta_min      4.77
_cell_volume                     2632.5(6)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_sigmaI/netI    0.0452
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7281
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.76
_diffrn_standards_decay_%        6.16
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.930
_exptl_absorpt_correction_T_max  0.5793
_exptl_absorpt_correction_T_min  0.4969
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'dark-brown                 '
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       'block                '
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.439
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.007
_refine_ls_goodness_of_fit_obs   1.027
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     856
_refine_ls_number_reflns         6890
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.013
_refine_ls_restrained_S_obs      1.028
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_obs          0.0420
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0646P)^2^+3.8471P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1225
_refine_ls_wR_factor_obs         0.1108
_reflns_number_observed          5637
_reflns_number_total             6892
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b004846l.txt
_cod_data_source_block           nickle_complex_2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0646P)^2^+3.8471P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0646P)^2^+3.8471P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P-1   '
_cod_database_code               7051352