Four-component intergrowth structures of the metal-ion cage complexes <i>fac</i>-(1,5,9,13,20-pentamethyl-3,7,11,15,18,22-hexaazabicyclo[7.7.7]tricosane)<i>M</i>^II^ diperchlorate hydrate, [<i>M</i>(C~22~H~48~N~6~)](ClO~4~)~2~.<i>x</i>H~2~O, <i>M</i> = Ni, Zn
Haller, Kenneth J.; Rae, A. David; Bygott, Alexia M. T.; Hockless, David C. R.; Ralph, Stephen F.; Geue, Rodney J.; Sargeson, Alan M.; Acta Crystallographica Section B 55 (1999) 380–388; doi:10.1107/S0108768198012968

data_2003166
_publ_section_title
;Four-component intergrowth structures of the metal-ion cage complexes
 <i>fac</i>-(1,5,9,13,20-pentamethyl-3,7,11,15,18,22-hexaazabicyclo[7.7.7]tricosane)<i>M</i>^II^
 diperchlorate hydrate, [<i>M</i>(C~22~H~48~N~6~)](ClO~4~)~2~.<i>x</i>H~2~O,
 <i>M</i> = Ni, Zn
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              380
_journal_page_last               388
_journal_paper_doi               10.1107/S0108768198012968
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac          '[Ni(C~22~H~48~N~6~)](ClO~4~)~2~.xH~2~O'
_chemical_formula_sum            'C22 H48 Cl2 N6 Ni O8'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 99.700(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1770(10)
_cell_length_b                   17.648(2)
_cell_length_c                   17.605(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      39.5
_cell_measurement_theta_min      31.9
_cell_volume                     3116.7(6)
_computing_cell_refinement       'PHILIPS PW1100/20 software'
_computing_data_collection       'MSC/AFC diffractometer control software'
_computing_data_reduction        XTAL_DIFDAT_ADSORB_SORTRF_ADDREF
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_structure_refinement  'RAELS96 (Rae, 1996)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'Rigaku AFC6R 4-circle diffractometer'
_diffrn_measurement_method       '\w/2\q scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9441
_diffrn_reflns_theta_max         60.50
_diffrn_reflns_theta_min         3.0
_diffrn_standards_decay_%        4.6
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.96
_exptl_absorpt_correction_T_max  0.733
_exptl_absorpt_correction_T_min  0.629
_exptl_absorpt_correction_type   'analytical  (de Meulenaer & Tompa, 1965)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.42
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1404.1
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_ls_extinction_coef       0.0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.91
_refine_ls_goodness_of_fit_obs   2.55
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         4104
_refine_ls_number_restraints     62
_refine_ls_R_factor_all          0.133
_refine_ls_R_factor_obs          0.074
_refine_ls_shift/esd_max         0.32
_refine_ls_shift/esd_mean        0.12
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w=1/[\s^2^(Fo)+(0.04Fo)^2^]
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.137
_refine_ls_wR_factor_obs         0.121
_reflns_number_observed          4104
_reflns_number_total             9441
_reflns_observed_criterion       >3sigma(I)
_cod_data_source_file            ta0004.cif
_cod_data_source_block           Ni
_cod_depositor_comments
;
 Adding _atom_site_type_symbol label and values.

 Antanas Vaitkus
 2013-04-08

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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)+(0.04Fo)^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)+(0.04Fo)^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3117.0(10)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C22 H48 Cl2 N6 O8 Ni'
_cod_database_code               2003166
_cod_database_fobs_code          2003166