Synthesis and Structural Characterization of a Nonplanar Neutral [36]Metallacrown-12 Nickel Compound [Ni(C13H9N3O2)(CH3OH)]12
Yan Bai; Dong-bin Dang; Chun-ying Duan; You Song; Qing-jin Meng; Inorganic Chemistry 44 (2005) 5972–5974; doi:10.1021/ic0506254

data_4309453
_publ_contact_author_address
;
Coordination Chemistry Institute
The State Key Laboratory of Coordinaiton Chemistry
Nanjing University , Nanjing 210093
P. R. China
;
_publ_contact_author_email       duancy@nju.edu.cn
_publ_contact_author_fax         '00 86 25 8331 4502'
_publ_contact_author_name        'Dr. Duan Chun-ying'
_publ_contact_author_phone       '00 86 25 8359 7006'
_publ_section_title
;
Synthesis and Structural Characterization of a Nonplanar Neutral
[36]Metallacrown-12 Nickel Compound [Ni(C13H9N3O2)(CH3OH)]12
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5972
_journal_page_last               5974
_journal_paper_doi               10.1021/ic0506254
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C185 H226 N36 Ni12 O54'
_chemical_formula_weight         4522.32
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 103.06(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   20.095(19)
_cell_length_b                   24.17(2)
_cell_length_c                   24.02(2)
_cell_measurement_reflns_used    4752
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.67
_cell_measurement_theta_min      2.26
_cell_volume                     11365(17)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.913
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0865
_diffrn_reflns_av_sigmaI/netI    0.1708
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            36648
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    1.048
_exptl_absorpt_correction_T_max  0.9156
_exptl_absorpt_correction_T_min  0.8786
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4712
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.753
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1227
_refine_ls_number_reflns         18306
_refine_ls_number_restraints     734
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1733
_refine_ls_R_factor_gt           0.0708
_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^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1560
_refine_ls_wR_factor_ref         0.1721
_reflns_number_gt                7296
_reflns_number_total             18306
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0506254si20050603_020339.cif
_cod_data_source_block           complex_1
_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 
;
_cod_original_cell_volume        11367(18)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4309453