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_7027144
_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 H18 Cl N2 Ni S3,Cl,H2 O'
_chemical_formula_structural     'C18 H18 Cl N2 Ni S3,Cl,H2 O'
_chemical_formula_sum            'C18 H20 Cl2 N2 Ni O S3'
_chemical_formula_weight         506.15
_chemical_melting_point          ?
_chemical_name_systematic
; 
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                99.226(14)
_cell_angle_beta                 117.279(13)
_cell_angle_gamma                109.407(13)
_cell_formula_units_Z            2
_cell_length_a                   10.972(3)
_cell_length_b                   11.472(2)
_cell_length_c                   10.264(2)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      24.96
_cell_measurement_theta_min      23.15
_cell_volume                     1004.9(5)
_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_type  '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    20.0980
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3543
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.555
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.842
_exptl_absorpt_correction_type   'empirical via \y scans'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.054
_refine_ls_goodness_of_fit_obs   1.176
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         3543
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.087
_refine_ls_restrained_S_obs      1.216
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_obs          0.0442
_refine_ls_shift/esd_max         -0.015
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0829P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1284
_refine_ls_wR_factor_obs         0.1238
_reflns_number_observed          2707
_reflns_number_total             3543
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            808062csup1.cif
_cod_data_source_block           compoundV
_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 
;
_cod_original_cell_volume        1004.9(4)
_cod_database_code               7027144