Formation and Dissociation Kinetics and Crystal Structures of Nickel(II)-Macrocyclic Tetrathiaether Complexes in Acetonitrile. Comparison to Nickel(II)-Macrocyclic Tetramines
Chandrika P. Kulatilleke; Scott N. Goldie; Mary Jane Heeg; L. A. Ochrymowycz; D. B. Rorabacher; Inorganic Chemistry 39 (2000) 1444–1453; doi:10.1021/ic991019+

data_4327642
_publ_section_title
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 Formation and Dissociation Kinetics and Crystal Structures of
 Nickel(II)-Macrocyclic Tetrathiaether Complexes in Acetonitrile.
 Comparison to Nickel(II)-Macrocyclic Tetramines
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1444
_journal_page_last               1453
_journal_paper_doi               10.1021/ic991019+
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C18 H32 Cl2 Ni O8 S4'
_chemical_formula_weight         634.29
_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                83.428(2)
_cell_angle_beta                 76.6390(10)
_cell_angle_gamma                87.6770(10)
_cell_formula_units_Z            1
_cell_length_a                   7.3849(6)
_cell_length_b                   8.8365(7)
_cell_length_c                   9.7503(8)
_cell_measurement_reflns_used    2722
_cell_measurement_temperature    295(2)
_cell_volume                     614.92(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'Bruker P4/CCD'
_diffrn_measurement_method       'SMART CCD'
_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  0.016
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4350
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    1.389
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_description       plate
_exptl_crystal_F_000             330
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       0.0000(19)
_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   0.971
_refine_ls_goodness_of_fit_obs   1.032
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         2761
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_restrained_S_obs      1.032
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_obs          0.0310
_refine_ls_shift/esd_max         -1.546
_refine_ls_shift/esd_mean        0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0555P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0823
_refine_ls_wR_factor_obs         0.0773
_reflns_number_observed          2226
_reflns_number_total             2763
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9910192B_3.cif
_cod_data_source_block           pler
_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^)+(0.0555P)^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^)+(0.0555P)^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_database_code               4327642