A new heterotrinuclear macrocyclic complex: bis(μ-diethyl 5,6,7,8,15,16-hexahydro-6,7-dioxo-5,8,14,17-tetraazadibenzo[<i>a</i>,<i>g</i>]cyclotetradecine-13,18-dicarboxylato)-1κ^4^<i>N</i>:2κ^2^<i>O</i>^6^,<i>O</i>^7^;2κ<i>O</i>^6^,<i>O</i>^7^:3κ^4^<i>N</i>-dimethanoldinickel(II)zinc(II) bis(perchlorate)
Li, Xiao-Zeng; He, Jun-Hong; Zhang, Wen-Qin; Liu, Bao-Lin; Acta Crystallographica Section E 61 (2005) m2018–m2020; doi:10.1107/S160053680502828X

data_2206966
_publ_section_title
;A new heterotrinuclear macrocyclic complex: bis(\m-diethyl
 5,6,7,8,15,16-hexahydro-6,7-dioxo-5,8,14,17-tetraazadibenzo[<i>a</i>,<i>g</i>]cyclotetradecine-13,18-dicarboxylato)-1\k^4^<i>N</i>:2\k^2^<i>O</i>^6^,<i>O</i>^7^;2\k<i>O</i>^6^,<i>O</i>^7^:3\k^4^<i>N</i>-dimethanoldinickel(II)zinc(II)
 bis(perchlorate)
;
_journal_coeditor_code           HG6213
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2018
_journal_page_last               m2020
_journal_paper_doi               10.1107/S160053680502828X
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac
'[Ni2 Zn (C24 H22 N4 O6)2 (C H4 O)2] (Cl O4)2'
_chemical_formula_moiety         'C50 H52 N8 Ni2 O14 Zn 2+ , 2Cl O4 -'
_chemical_formula_sum            'C50 H52 Cl2 N8 Ni2 O22 Zn'
_chemical_formula_weight         1370.69
_chemical_name_systematic
;
bis(\m-diethyl
5,6,7,8,15,16-hexahydro-6,7-dioxo-5,8,14,17-
tetraazadibenzo[a,g]cyclotetradecine-13,18-
dicarboxylate)-1\k^4^N:2\k^2^O^6^,O^7^;2\kO^6^,O^7^:3\k^4^N-
dimethanoldinickel(II)zinc(II) bis(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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 99.308(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.4582(16)
_cell_length_b                   12.8031(19)
_cell_length_c                   21.161(3)
_cell_measurement_reflns_used    4578
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      2.52
_cell_volume                     2796.1(7)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0223
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            14921
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.87
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.276
_exptl_absorpt_correction_T_max  0.836
_exptl_absorpt_correction_T_min  0.674
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.573
_refine_diff_density_min         -0.455
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         4941
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0666P)^2^+2.4619P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0997
_refine_ls_wR_factor_ref         0.1055
_reflns_number_gt                4033
_reflns_number_total             4941
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hg6213.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 'Monoclinic' changed to 'monoclinic'
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_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2206966
_cod_database_fobs_code          2206966