Acetato[μ-10,21-dibutyl-3,6,14,17-tetrazatricyclo[17.3.1.1^8,12^]tetracosa-1(23),2,6,8,10,12(24),13,17,19,21-decaene-23,24-diolato(2‒)-κ^4^<i>N</i>^3^,<i>N</i>^6^,<i>O</i>^23^,<i>O</i>^24^:κ^4^<i>N</i>^14^,<i>N</i>^17^,<i>O</i>^23^,<i>O</i>^24^]dinickel(II) perchlorate acetonitrile hemisolvate
Hong Zhou; Zhi-Quan Pan; Yan-Jiao Zhang; Acta Crystallographica Section E 62 (2006) m2442–m2444; doi:10.1107/S1600536806034751

data_2210842
_publ_section_title
;Acetato[\m-10,21-dibutyl-3,6,14,17-tetrazatricyclo[17.3.1.1^8,12^]tetracosa-1(23),2,6,8,10,12(24),13,17,19,21-decaene-23,24-diolato(2--)-\k^4^<i>N</i>^3^,<i>N</i>^6^,<i>O</i>^23^,<i>O</i>^24^:\k^4^<i>N</i>^14^,<i>N</i>^17^,<i>O</i>^23^,<i>O</i>^24^]dinickel(II)
 perchlorate acetonitrile hemisolvate
;
_journal_coeditor_code           YA2023
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2442
_journal_page_last               m2444
_journal_paper_doi               10.1107/S1600536806034751
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C30 H37 N4 Ni2 O4 +, Cl O4 -, 0.5C2 H3 N'
_chemical_formula_moiety         'C30 H37 N4 Ni2 O4 +, Cl O4 -, 0.5C2 H3 N'
_chemical_formula_sum            'C31 H38.5 Cl N4.5 Ni2 O8'
_chemical_formula_weight         755.01
_chemical_name_systematic
;Acetato[\m-10,21-dibutyl-3,6,14,17-tetrazatricyclo[17.3.1.1^(8,12)^]tetracosa-
1(23),2,6,8,10,12(24),13,17,19,21-decaene-23,24-diolato(2-)-
\k^4^N^3^,N^6^,O^23^,O^24^:\k^4^N^14^,N^17^,O^23^,O^24^]dinickel(II)
perchlorate
 acetonitrile hemisolvate
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 116.8750(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   31.353(2)
_cell_length_b                   11.2316(7)
_cell_length_c                   21.2808(14)
_cell_measurement_reflns_used    9027
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.3
_cell_measurement_theta_min      2.4
_cell_volume                     6684.5(7)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.048
_diffrn_reflns_av_sigmaI/netI    0.043
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            28559
_diffrn_reflns_theta_full        26.0
_diffrn_reflns_theta_max         26.0
_diffrn_reflns_theta_min         1.9
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.262
_exptl_absorpt_correction_T_max  0.786
_exptl_absorpt_correction_T_min  0.703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'block cut from needle'
_exptl_crystal_F_000             3144
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.26
_refine_diff_density_min         -0.40
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.06
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         6572
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.06
_refine_ls_R_factor_all          0.060
_refine_ls_R_factor_gt           0.045
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.05P)^2^+1.55P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.098
_refine_ls_wR_factor_ref         0.101
_reflns_number_gt                5169
_reflns_number_total             6572
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ya2023.cif
_cod_data_source_block           I
_cod_original_cell_volume        6684.6(7)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2210842
_cod_database_fobs_code          2210842