Synthesis, structure and optical limiting effect of two new nickel complexes containing strongly bound geometrically fixed multi‐sulfur 1,2‐dithiolene ligands showing remarkable near‐IR absorption
Bai, Jun‐Feng; Zuo, Jing‐Lin; Tan, Wei‐Lian; Ji, Wei; Shen, Zhen; Fun, Hoong‐Kun; Chinnakali, Kandasamy; Abdul Razak, Ibrahim; You, Xiao‐Zeng; Che, Chi‐Ming; Journal of Materials Chemistry 9 (1999) 2419–; doi:10.1039/a902295c

data_7213064
_publ_section_title
;
 Synthesis, structure and optical limiting effect of two new nickel
 complexes containing strongly bound geometrically fixed
 multi&#x2010;sulfur 1,2&#x2010;dithiolene ligands showing remarkable
 near&#x2010;IR absorption
;
_journal_issue                   10
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              2419
_journal_paper_doi               10.1039/a902295c
_journal_volume                  9
_journal_year                    1999
_chemical_formula_sum            'C16 H20 Ni S8'
_chemical_formula_weight         527.51
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 107.709(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.171(2)
_cell_length_b                   5.2299(7)
_cell_length_c                   16.567(2)
_cell_measurement_reflns_used    4085
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.0
_cell_measurement_theta_min      1.50
_cell_volume                     1004.6(3)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1994)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1996)'
_computing_publication_material
; SHELXTL (Sheldrick, 1996)
  PARST (Nardelli, 1995) 
;
_computing_structure_refinement  'SHELXTL (Sheldrick, 1996)'
_computing_structure_solution    'SHELXTL (Sheldrick, 1996)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device
;
Siemens SMART CCD area detector diffractometer 
;
_diffrn_measurement_method       '\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  0.0172
_diffrn_reflns_av_sigmaI/netI    0.0194
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5078
_diffrn_reflns_theta_max         24.74
_diffrn_reflns_theta_min         3.51
_exptl_absorpt_coefficient_mu    1.796
_exptl_absorpt_correction_T_max  0.789
_exptl_absorpt_correction_T_min  0.633
_exptl_absorpt_correction_type   'empirical using SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            'bluish black'
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.175
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.060
_refine_ls_goodness_of_fit_obs   1.074
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         1706
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_restrained_S_obs      1.074
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_obs          0.0211
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0249P)^2^+0.4578P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0528
_refine_ls_wR_factor_obs         0.0510
_reflns_number_observed          1563
_reflns_number_total             1706
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            902295csup1.cif
_cod_data_source_block           bjf3m
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0249P)^2^+0.4578P] 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^)+(0.0249P)^2^+0.4578P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1004.6(2)
_cod_database_code               7213064