Mixed aza‒thia crowns containing the 1,10-phenanthroline sub-unit. Substitution reactions in [NiL(MeCN)][BF4]2 {L = 2,5,8-trithia[9](2,9)-1,10-phenanthrolinophane} †
Blake, Alexander J.; Casabò, Jaume; Devillanova, Francesco A.; Escriche, Lluis; Garau, Alessandra; Isaia, Francesco; Lippolis, Vito; Kivekas, Raikko; Muns, Vincens; Schröder, Martin; Sillanpää, Reijo; Verani, Gaetano; Journal of the Chemical Society, Dalton Transactions  (1999) 1085–; doi:10.1039/a808062c

data_7027143
_publ_section_title
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 Mixed aza--thia crowns containing the 1,10-phenanthroline sub-unit.
 Substitution reactions in [NiL(MeCN)][BF4]2
 {L&#x2005;=&#x2005;2,5,8-trithia[9](2,9)-1,10-phenanthrolinophane}&#x200A;&#x2020;
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_journal_issue                   7
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1085
_journal_paper_doi               10.1039/a808062c
_journal_year                    1999
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C18 H20 N2 Ni O S3,(Cl O4)2,H2 O'
_chemical_formula_structural     'C18 H20 N2 Ni O S3,(Cl O4)2,H2 O'
_chemical_formula_sum            'C18 H22 Cl2 N2 Ni O10 S3'
_chemical_formula_weight         652.17
_chemical_melting_point          ?
_chemical_name_systematic
; 
 ? 
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_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.830(2)
_cell_length_b                   22.432(2)
_cell_length_c                   14.2490(12)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      20.48
_cell_measurement_theta_min      16.78
_cell_volume                     5059.8(9)
_computing_cell_refinement
;
MSC/AFC5S Control Program (Molecular Structure Corporation, 1995)
;
_computing_data_collection
;
MSC/AFC5S Control Program (Molecular Structure Corporation, 1995)
;
_computing_data_reduction
;
TEXSAN (Molecular Structure Corporation, 1989)
;
_computing_molecular_graphics    'ORTEP II (Johnson, 1976)'
_computing_publication_material  'SHELXL-92 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-92 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measurement_device       'Rigaku AFC5S'
_diffrn_measurement_method       \w--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1205
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4459
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.82
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.282
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.909
_exptl_absorpt_correction_type   'empirical via \y scans'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2672
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.056
_refine_ls_goodness_of_fit_obs   1.171
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         4442
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.176
_refine_ls_restrained_S_obs      1.169
_refine_ls_R_factor_all          0.1724
_refine_ls_R_factor_obs          0.0657
_refine_ls_shift/esd_max         0.004
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+38.9000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1692
_refine_ls_wR_factor_obs         0.1170
_reflns_number_observed          2302
_reflns_number_total             4459
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            808062csup1.cif
_cod_data_source_block           compoundIV
_cod_depositor_comments
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The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

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^)+(0.0000P)^2^+38.9000P] 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^)+(0.0000P)^2^+38.9000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7027143