(<i>C</i>-<i>rac</i>-5,5,7,12,12,14-Hexamethyl-1,4,8,11-tetraazacyclotetradecane-κ^4^<i>N</i>)(nicotinato-<i>O</i>,<i>O</i>')nickel(II) perchlorate
Basiuk, Elena V.; Basiuk, Vladimir A.; Hernández-Ortega, Simón; Martínez-García, Marcos; Saniger-Blesa, José-Manuel; Acta Crystallographica Section C 57 (2001) 553–555; doi:10.1107/S010827010100333X

data_2011953
_publ_section_title
;(<i>C</i>-<i>rac</i>-5,5,7,12,12,14-Hexamethyl-1,4,8,11-tetraazacyclotetradecane-\k^4^<i>N</i>)(nicotinato-<i>O</i>,<i>O</i>')nickel(II)
 perchlorate
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              553
_journal_page_last               555
_journal_paper_doi               10.1107/S010827010100333X
_journal_volume                  57
_journal_year                    2001
_chemical_formula_iupac          '[Ni(C16 H36 N4)(C6 H4 N O2)], (Cl O4)'
_chemical_formula_moiety         'C22 H40 N5 Ni O2 + , Cl O4 -'
_chemical_formula_sum            'C22 H40 Cl N5 Ni O6'
_chemical_formula_weight         564.75
_chemical_name_common            '[Ni(rac-Me6[14]aneN4)(nicotinato)]ClO4'
_chemical_name_systematic
;
(Nicotinato-O,O')(C-rac-5,5,7,12,12,14-hexamethyl-1,4,8,11-
tetraazacyclotetradecane-N,N',N'',N''')nickel(II) perchlorate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 91.330(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.474(2)
_cell_length_b                   13.221(2)
_cell_length_c                   20.288(3)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.5
_cell_measurement_theta_min      3.9
_cell_volume                     2808.7(8)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens 1994)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    'XP in SHELXTL/PC (Sheldrick 1990)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full .954
_diffrn_measured_fraction_theta_max .954
_diffrn_measurement_device_type  'Siemens P4/PC'
_diffrn_measurement_method       \w
_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  .057
_diffrn_reflns_av_sigmaI/netI    .083
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            5239
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .829
_exptl_absorpt_correction_T_max  .879
_exptl_absorpt_correction_T_min  .755
_exptl_absorpt_correction_type   \y-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          .36
_exptl_crystal_size_mid          .24
_exptl_crystal_size_min          .16
_refine_diff_density_max         .70
_refine_diff_density_min         -.35
_refine_ls_extinction_coef       .00184(16)
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   .959
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         4950
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      .959
_refine_ls_R_factor_all          .087
_refine_ls_R_factor_gt           .046
_refine_ls_shift/su_max          .009
_refine_ls_shift/su_mean         .001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.025P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .100
_reflns_number_gt                2980
_reflns_number_total             4950
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            da1165.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.025P)^2^] 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^)+(0.025P)^2^] 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/c'
_cod_database_code               2011953
_cod_database_fobs_code          2011953