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_4321024
_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            'C46 H48 Cl4 N4 Ni2 O8'
_chemical_formula_weight         1044.12
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      1
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_cell_angle_alpha                106.29(2)
_cell_angle_beta                 91
_cell_angle_gamma                68
_cell_formula_units_Z            1
_cell_length_a                   10.366(4)
_cell_length_b                   12.170(3)
_cell_length_c                   10.021(2)
_cell_measurement_reflns_used    16
_cell_measurement_temperature    299.2
_cell_measurement_theta_max      11.4
_cell_measurement_theta_min      10.2
_cell_volume                     1119.6(6)
_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      0.02525
_diffrn_orient_matrix_UB_12      0.09135
_diffrn_orient_matrix_UB_13      0.03062
_diffrn_orient_matrix_UB_21      0.08200
_diffrn_orient_matrix_UB_22      0.00993
_diffrn_orient_matrix_UB_23      0.05888
_diffrn_orient_matrix_UB_31      0.05864
_diffrn_orient_matrix_UB_32      0.00739
_diffrn_orient_matrix_UB_33      0.08048
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Xray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.03297
_diffrn_reflns_av_sigmaI/netI    0.082
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       11
_diffrn_reflns_number            3564
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.83
_diffrn_standards_decay_%        38.80
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.132
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.799
_exptl_absorpt_correction_type   '\y scans (North,Phillips & Matthews, 1968)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'rectangular plate'
_exptl_crystal_F_000             540.00
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
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_refine_diff_density_min         0.43
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.740
_refine_ls_goodness_of_fit_ref   1.940
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     354
_refine_ls_number_reflns         2385
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1092
_refine_ls_R_factor_gt           0.0520
_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) + 0.00007|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0580
_refine_ls_wR_factor_ref         0.0530
_reflns_number_gt                2385
_reflns_number_total             3326
_reflns_threshold_expression     I>2.00\s(I)
_cod_data_source_file            ic990935k_2.cif
_cod_data_source_block           '_zl0383'
_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        1126.3(5)
_cod_original_sg_symbol_H-M      'P 1        '
_cod_original_formula_sum        'C46 H48 Cl4 N4 O8 Ni2 '
_cod_database_code               4321024