Synthesis and structure of cyclen hydroxylamine ligands and their zinc(II) complexes
Roland Reichenbach-Klinke; Manfred Zabel; Burkhard König; Dalton Trans.  (2003) 141–145; doi:10.1039/b207571g

data_7012119
_publ_section_title
;
 Synthesis and structure of cyclen hydroxylamine ligands and their
 zinc(II) complexes
;
_journal_issue                   1
_journal_name_full               'Dalton Trans.'
_journal_page_first              141
_journal_page_last               145
_journal_paper_doi               10.1039/b207571g
_journal_year                    2003
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C8 H20 Br N4 O Zn, Cl O4'
_chemical_formula_structural     'C8 H20 Br N4 O Zn, Cl O4'
_chemical_formula_sum            'C8 H20 Br Cl N4 O5 Zn'
_chemical_formula_weight         433.02
_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_date             'Apr 12 16:50:48 2002'
_audit_creation_method           'PLATON <TABLE ACC> option'
_audit_update_record
;
?
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9049(5)
_cell_length_b                   12.2325(8)
_cell_length_c                   14.0969(11)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    173
_cell_measurement_theta_max      25.77
_cell_measurement_theta_min      2.71
_cell_volume                     1535.56(18)
_computing_cell_refinement       'STOE (1998)'
_computing_data_collection       'STOE (1998)'
_computing_data_reduction        'STOE (1998)'
_computing_molecular_graphics    'PLATON (Spek, 1990)'
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare, 1993)'
_diffrn_ambient_temperature      173(1)
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device_type  'STOE-IPDS diffractometer'
_diffrn_measurement_method       rotation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11144
_diffrn_reflns_reduction_process
;
?
;
_diffrn_reflns_theta_full        25.77
_diffrn_reflns_theta_max         25.77
_diffrn_reflns_theta_min         2.71
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.398
_exptl_absorpt_correction_T_max  0.3722
_exptl_absorpt_correction_T_min  0.1585
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'numerical from crystal shape (X-SHAPE, X-RED. STOE, 1996)'
_exptl_crystal_colour            'translucent colourless'
_exptl_crystal_density_diffrn    1.873
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.525
_exptl_crystal_size_mid          0.454
_exptl_crystal_size_min          0.375
_refine_diff_density_max         1.248
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.120
_refine_ls_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.45(1)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2904
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0651P)^2^+0.1652P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0843
_refine_ls_wR_factor_ref         0.0850
_reflns_number_gt                2754
_reflns_number_total             2904
_reflns_threshold_expression     I>4\\s(I)
_cod_data_source_file            b207571g.txt
_cod_data_source_block           b043
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               7012119