Synthesis, Characterization, and Structure of Macrocyclic Mono- and C2-Symmetric, Binuclear Nickel Calixsalen Complexes
Zengmin Li; Chet Jablonski; Inorganic Chemistry 39 (2000) 2456–2461; doi:10.1021/ic990935k

data_4321025
_publ_section_title
;
 Synthesis, Characterization, and Structure of Macrocyclic Mono- and
 C2-Symmetric, Binuclear Nickel Calixsalen Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2456
_journal_page_last               2461
_journal_paper_doi               10.1021/ic990935k
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C60.7 H83.4 Cl1.4 N5 Ni2 O4'
_chemical_formula_weight         1114.19
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.531(2)
_cell_length_b                   22.819(3)
_cell_length_c                   13.373(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    299.2
_cell_measurement_theta_max      29.8
_cell_measurement_theta_min      27.4
_cell_volume                     5960.1(11)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction
'teXsan for Windows version 1.06 (MSC, 1997-1999)'
_computing_publication_material
'teXsan for Windows version 1.06 (MSC, 1997-1999)'
_computing_structure_refinement
'teXsan for Windows version 1.06 (MSC, 1997-1999)'
_computing_structure_solution
;
SHELXS86 (Sheldrick, 1985)
;
_diffrn_ambient_temperature      299.2
_diffrn_measurement_device       'Rigaku AFC6S'
_diffrn_measurement_method       \w2\q
_diffrn_orient_matrix_UB_11      0.00264
_diffrn_orient_matrix_UB_12      0.04199
_diffrn_orient_matrix_UB_13      0.02103
_diffrn_orient_matrix_UB_21      0.00011
_diffrn_orient_matrix_UB_22      0.01235
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_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
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_diffrn_radiation_wavelength     1.5418
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_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4946
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_diffrn_reflns_theta_min         2.98
_diffrn_standards_decay_%        1.86
_diffrn_standards_interval_count 150
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_exptl_crystal_colour            red
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_exptl_crystal_density_meas      ?
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_refine_diff_density_min         0.61
_refine_ls_extinction_coef       0.00000024(2)
_refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.'
_refine_ls_extinction_method     'Zachariasen (1967)'
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_refine_ls_goodness_of_fit_ref   3.600
_refine_ls_hydrogen_treatment    noref
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_refine_ls_R_factor_gt           0.0670
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0002
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00001|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0670
_refine_ls_wR_factor_ref         0.0650
_reflns_number_gt                3752
_reflns_number_total             4946
_reflns_threshold_expression     I>2.00\s(I)
_cod_data_source_file            ic990935k_3.cif
_cod_data_source_block           '_zl0405_________________'
_cod_depositor_comments
;
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        5960(1)
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        'C60.70 H83.40 Cl1.40 N5 O4 Ni2 '
_cod_database_code               4321025