Ni^II^ and Zn^II^ complexes of the hexadentate macrocyclic ligand <i>cis</i>-6,13-dimethyl-1,4,8,11-tetraazacyclotetradecane-6,13-diamine
Bernhardt, Paul V.; Acta Crystallographica Section C 56 (2000) 744–746; doi:10.1107/S0108270100003930

data_2011109
_publ_section_title
;
 Ni^II^ and Zn^II^ complexes of the hexadentate macrocyclic ligand
 <i>cis</i>-6,13-dimethyl-1,4,8,11-tetraazacyclotetradecane-6,13-diamine
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              744
_journal_page_last               746
_journal_paper_doi               10.1107/S0108270100003930
_journal_volume                  56
_journal_year                    2000
_chemical_formula_moiety         '[Ni (C12 H30  N6 )] , 2ClO4'
_chemical_formula_sum            'C12 H30 Cl2 N6 Ni O8'
_chemical_formula_weight         516.03
_chemical_name_systematic
;
cis(6,13-dimethyl-1,4,8,11-tetraazacyclotetradecan-6,13-diamine)nickel(II)
perchlorate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 113.09(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.198(4)
_cell_length_b                   12.7710(10)
_cell_length_c                   9.880(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      10
_cell_volume                     1067.6(7)
_computing_cell_refinement       'SET4 in CAD-4 Manual'
_computing_data_collection       'CAD-4 Manual (Enraf-Nonius, 1988)'
_computing_data_reduction        'XTAL3.2 (Hall, 1992)'
_computing_molecular_graphics    'PLATON (Spek, 1990)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full .999
_diffrn_measured_fraction_theta_max .999
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       '\w-2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0258
_diffrn_reflns_av_sigmaI/netI    .0168
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2097
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.24
_diffrn_standards_decay_%        'less than 5'
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.210
_exptl_absorpt_correction_T_max  .546
_exptl_absorpt_correction_T_min  .404
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             540
_exptl_crystal_size_max          .50
_exptl_crystal_size_mid          .50
_exptl_crystal_size_min          .50
_refine_diff_density_max         .574
_refine_diff_density_min         -.832
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   .03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         1971
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          .0460
_refine_ls_R_factor_gt           .0436
_refine_ls_shift/su_max          .000
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0981P)^2^+0.2008P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .1173
_reflns_number_gt                1892
_reflns_number_total             1971
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fg1588.cif
_cod_data_source_block           I
_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 'calc w =
1/[\s^2^(Fo^2^)+(0.0981P)^2^+0.2008P] 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^)+(0.0981P)^2^+0.2008P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2011109
_cod_database_fobs_code          2011109