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_7027145
_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            'C23 H23 B2 F8 N3 Ni S3'
_chemical_formula_weight         669.95
_chemical_name_systematic
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 ? 
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_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.27(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.270(20)
_cell_length_b                   13.500(20)
_cell_length_c                   18.270(20)
_cell_measurement_reflns_used    43
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      12.5
_cell_volume                     2533(7)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      220(2)
_diffrn_measurement_device       'Stoe Stadi-4'
_diffrn_measurement_method       omega/theta
_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  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0518
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4986
_diffrn_reflns_theta_max         25.87
_diffrn_reflns_theta_min         2.69
_exptl_absorpt_coefficient_mu    1.094
_exptl_absorpt_correction_T_max  0.839
_exptl_absorpt_correction_T_min  0.764
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.757
_exptl_crystal_description       column
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.997
_refine_diff_density_min         -1.452
_refine_diff_density_rms         0.177
_refine_ls_extinction_coef       0.0000(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.066
_refine_ls_goodness_of_fit_obs   1.000
_refine_ls_hydrogen_treatment    riding/model
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         4544
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_restrained_S_obs      1.000
_refine_ls_R_factor_all          0.1481
_refine_ls_R_factor_obs          0.1143
_refine_ls_shift/esd_max         0.010
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2061P)^2^+49.1654P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3629
_refine_ls_wR_factor_obs         0.2975
_reflns_number_observed          3762
_reflns_number_total             4590
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            808062csup1.cif
_cod_data_source_block           nipnpy
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.2061P)^2^+49.1654P] 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^)+(0.2061P)^2^+49.1654P] 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_cell_volume        2533.0(68)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7027145