Synthesis and Structural Characterization of a Novel Mixed-Valent CuIICuICuII Triangular Metallomacrocycle Using an Imine-Based Rigid Ligand
Guo Dong; Qian Chun-qi; Duan Chun-ying; Pang Ke-liang; Meng Qing-jin; Inorganic Chemistry 42 (2003) 2024–2030; doi:10.1021/ic0260668

data_4313390
_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 25 331 4502'
_publ_contact_author_name        'Dr. Duan Chun-ying'
_publ_contact_author_phone       '00 86 25 359 7006'
_publ_section_title
;
 Synthesis and Structural Characterization of a Novel Mixed-Valent
 CuIICuICuII Triangular Metallomacrocycle Using an Imine-Based Rigid
 Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2024
_journal_page_last               2030
_journal_paper_doi               10.1021/ic0260668
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C81 H71 Cu3 N6 O11'
_chemical_formula_weight         1495.06
_chemical_name_systematic
; 
 ? 
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.917(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.687(10)
_cell_length_b                   24.161(13)
_cell_length_c                   18.484(10)
_cell_measurement_reflns_used    574
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.297
_cell_measurement_theta_min      2.155
_cell_volume                     7687(7)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_reflns_av_R_equivalents  0.2291
_diffrn_reflns_av_sigmaI/netI    0.5067
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30319
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    0.884
_exptl_absorpt_correction_T_max  0.838
_exptl_absorpt_correction_T_min  0.767
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown-black
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3096
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.917
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     928
_refine_ls_number_reflns         10026
_refine_ls_number_restraints     643
_refine_ls_restrained_S_all      0.908
_refine_ls_R_factor_all          0.2919
_refine_ls_R_factor_gt           0.0758
_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 
 [0.00000+1.00000exp(3.00(sin\q/\l)^2^)]/ 
   [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0000P)^2^+0.0000sin\q/\l] 
 where P = 0.33333Fo^2^ + 0.66667Fc^2^ 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1272
_refine_ls_wR_factor_ref         0.1715
_reflns_number_gt                2245
_reflns_number_total             10026
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0260668si20021217_080554.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 the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4313390