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_4327640
_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           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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            4
_cell_length_a                   12.3856(6)
_cell_length_b                   12.8029(7)
_cell_length_c                   16.4921(9)
_cell_measurement_reflns_used    7712
_cell_measurement_temperature    295(2)
_cell_volume                     2615.2(2)
_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  0.046
_diffrn_reflns_av_sigmaI/netI    0.0594
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            18298
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    1.306
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_description       chunks
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_coef       0.0000(4)
_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   0.945
_refine_ls_goodness_of_fit_obs   1.057
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         6114
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.964
_refine_ls_restrained_S_obs      1.057
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_obs          0.0476
_refine_ls_shift/esd_max         -3.948
_refine_ls_shift/esd_mean        0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0737P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1265
_refine_ls_wR_factor_obs         0.1132
_reflns_number_observed          4145
_reflns_number_total             6117
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9910192B_1.cif
_cod_data_source_block           dine
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0737P)^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^)+(0.0737P)^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               4327640