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_7027147
_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_formula_sum            'C20 H21 B F4 N4 Ni O2 S4'
_chemical_formula_weight         623.17
_chemical_name_systematic
; 
 ? 
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_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 110.749(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.606(2)
_cell_length_b                   12.2919(6)
_cell_length_c                   13.671(2)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.5
_cell_volume                     2452.4(5)
_computing_cell_refinement       'MADNES ( ???)'
_computing_data_collection       'MADNES ( ???)'
_computing_structure_refinement  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_solution    'SHELXS-96 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.820
_diffrn_measured_fraction_theta_max 0.820
_diffrn_measurement_device_type  'Enraf-Nonius FAST'
_diffrn_measurement_method       'area detector 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  0.0673
_diffrn_reflns_av_sigmaI/netI    0.0858
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9967
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    1.190
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.538
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.826
_refine_ls_hydrogen_treatment    riding/model
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         3751
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.826
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0266P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0691
_refine_ls_wR_factor_ref         0.0715
_reflns_number_gt                2730
_reflns_number_total             3751
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            808062csup1.cif
_cod_data_source_block           niscpn
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0266P)^2^+0.0000P] 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^)+(0.0266P)^2^+0.0000P] 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      P2(1)/c
_cod_database_code               7027147