[μ-10,21-Di-<i>tert</i>-butyl-4(<i>S</i>),5(<i>S</i>),15(<i>S</i>),16(<i>S</i>)-tetraphenyl-3,6,14,17-tetraazatricyclo[17.3.1.18,12]tetracosa-1(23),2,6,8,10,12(24),13,17,19,21-decaene-23,24-diolato](μ-ethylene glycol)dinickel(II) diperchlorate dihydrate
Wu, Jin-Cai; Li, Yi-Zhi; Tang, Ling; Tan, Min-Yu; Acta Crystallographica Section E 59 (2003) m494–m496; doi:10.1107/S1600536803012868

data_2202769
_publ_section_title
;[\m-10,21-Di-<i>tert</i>-butyl-4(<i>S</i>),5(<i>S</i>),15(<i>S</i>),16(<i>S</i>)-tetraphenyl-3,6,14,17-tetraazatricyclo[17.3.1.18,12]tetracosa-1(23),2,6,8,10,12(24),13,17,19,21-decaene-23,24-diolato](\m-ethylene
 glycol)dinickel(II) diperchlorate dihydrate
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m494
_journal_page_last               m496
_journal_paper_doi               10.1107/S1600536803012868
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac
'[Ni2 (C52 H50 N4 O2) (C2 H6 O2)] (Cl O4)2, 2H2 O'
_chemical_formula_moiety         'C54 H56 N4 Ni2 O4 2+, 2Cl O4 1-, 2H2 O'
_chemical_formula_sum            'C54 H60 Cl2 N4 Ni2 O14'
_chemical_formula_weight         1177.38
_chemical_name_systematic
;
 (R,R,R,R)10,21-Di-tert-butyl-4,5,15,16-tetraphenyl-3,6,14,17-tetraaza
 -tricyclo[17.3.1.18,12]tetracosa-1(23),2,6,8,10,12(24),13,17,
 19,21-decaene-23,24-diol ethane-1,2-diol dinuclear Nickel(II)
 diperchlorate bishydrate complex
;
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.536(3)
_cell_length_b                   11.536(3)
_cell_length_c                   43.015(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16.74
_cell_measurement_theta_min      2.21
_cell_volume                     5724(2)
_computing_cell_refinement       'CAD-4 SDP/VAX'
_computing_data_collection       'CAD-4 SDP/VAX (Enraf-Nonius, 1989)'
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1989)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0105
_diffrn_reflns_av_sigmaI/netI    0.0205
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            8048
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.83
_diffrn_standards_decay_%        3.95
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.817
_exptl_absorpt_correction_T_max  0.799
_exptl_absorpt_correction_T_min  0.750
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(XPREP; Bruker, 2000)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2456
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.577
_refine_ls_abs_structure_details 'Flack (1983), 2037 Friedel pairs'
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         5296
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0471
_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^)+(0.105P)^2^+1.99P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1583
_refine_ls_wR_factor_ref         0.1590
_reflns_number_gt                4763
_reflns_number_total             5296
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ob6245.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2202769
_cod_database_fobs_code          2202769