Solution and solid state structures of binuclear zinc(II) complexes of bis(pentadentate) ligands derived from bis(1,4,7-triazacyclononane) macrocycles
J. Brudenell, Suzanne; Spiccia, Leone; C. R. Hockless, David; R. T. Tiekink, Edward; Journal of the Chemical Society, Dalton Transactions  (1999) 1475–; doi:10.1039/a809946d

data_7027234
_publ_section_title
;
 Solution and solid state structures of binuclear zinc(II) complexes of
 bis(pentadentate) ligands derived from bis(1,4,7-triazacyclononane)
 macrocycles
;
_journal_issue                   9
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1475
_journal_paper_doi               10.1039/a809946d
_journal_year                    1999
_chemical_formula_sum            'C42 H64 Br2 Cl2 N10 O10 S2 Zn2'
_chemical_formula_weight         1294.62
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             1999-01-24
_audit_creation_method           'by teXsan v1.8'
_audit_update_record
;
?
;
_cell_angle_alpha                111.59(1)
_cell_angle_beta                 105.18(1)
_cell_angle_gamma                95.82(1)
_cell_formula_units_Z            1
_cell_length_a                   8.103(1)
_cell_length_b                   13.576(2)
_cell_length_c                   13.987(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      17.4
_cell_measurement_theta_min      13.7
_cell_volume                     1346.8(4)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1992-1997)'
_computing_publication_material  'teXsan (MSC, 1992-1997)'
_computing_structure_refinement  'teXsan (MSC, 1992-1997)'
_computing_structure_solution
;
SIR92 (Altomare, et. al. 1993)
;
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device_type  'Rigaku AFC6S'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.01226
_diffrn_orient_matrix_UB_12      -0.07505
_diffrn_orient_matrix_UB_13      -0.05478
_diffrn_orient_matrix_UB_21      -0.00015
_diffrn_orient_matrix_UB_22      0.02905
_diffrn_orient_matrix_UB_23      -0.05615
_diffrn_orient_matrix_UB_31      0.13052
_diffrn_orient_matrix_UB_32      0.01095
_diffrn_orient_matrix_UB_33      0.02118
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.01303
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5143
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.65
_diffrn_standards_decay_%        0.48
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.617
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.915
_exptl_absorpt_correction_type
;
\y scans (North,Phillips & Matthews, 1968)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             662.00
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.42
_refine_diff_density_min         -0.79
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   2.960
_refine_ls_goodness_of_fit_ref   3.449
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     317
_refine_ls_number_reflns         3415
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/esd_max         0.0060
_refine_ls_shift/esd_mean        0.2790
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00009|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0723
_refine_ls_wR_factor_ref         0.0702
_reflns_number_gt                3415
_reflns_number_total             4774
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            809946dsup1.cif
_cod_data_source_block           SB-9
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo) +
0.00009|Fo|^2^]' 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) + 0.00009|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1346.9(4)
_cod_original_sg_symbol_H-M      'P -1       '
_cod_original_formula_sum        'C42 H64 Br2 Cl2 N10 O10 S2 Zn2 '
_cod_database_code               7027234