Oligonuclear Copper Complexes of a Bioinspired Pyrazolate-Bridging Ligand: Synthesis, Structures, and Equilibria in Solution
Angelina Prokofieva; Alexander I. Prikhod'ko; Eva Anna Enyedy; Etelka Farkas; Walter Maringgele; Serhiy Demeshko; Sebastian Dechert; Franc Meyer; Inorganic Chemistry 46 (2007) 4298–4307; doi:10.1021/ic062434m

data_4307925
_publ_contact_author_address
; Institut f\"ur Anorganische Chemie
  Georg August Universit\"at G\"ottingen
  Tammannstra\&se 4
  D-37077 G\"ottingen
  Germany
;
_publ_contact_author_email       franc.meyer@chemie.uni-goettingen.de
_publ_contact_author_fax         49(551)393063
_publ_contact_author_name        'Prof. Dr. Franc Meyer'
_publ_contact_author_phone       49(551)393012
_publ_section_title
;
Oligonuclear Copper Complexes of a Bioinspired Pyrazolate-Bridging
Ligand: Synthesis, Structures, and Equilibria in Solution
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4298
_journal_page_last               4307
_journal_paper_doi               10.1021/ic062434m
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C27 H40 Cu2 N12 O2 2+, 2(Cl O4 -), C2 H3 N'
_chemical_formula_sum            'C29 H43 Cl2 Cu2 N13 O10'
_chemical_formula_weight         931.74
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 112.350(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.1991(9)
_cell_length_b                   16.9395(6)
_cell_length_c                   13.6063(8)
_cell_measurement_reflns_used    29113
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      24.81
_cell_measurement_theta_min      1.71
_cell_volume                     3879.5(3)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2002)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       \w
_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  0.0651
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            29113
_diffrn_reflns_theta_full        24.81
_diffrn_reflns_theta_max         24.81
_diffrn_reflns_theta_min         1.71
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.305
_exptl_absorpt_correction_T_max  0.7515
_exptl_absorpt_correction_T_min  0.5886
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2002)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.001(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         6527
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0287
_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^)+(0.0450P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0674
_refine_ls_wR_factor_ref         0.0682
_reflns_number_gt                6123
_reflns_number_total             6527
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062434msi20061219_032313_2.cif
_cod_data_source_block           1a
_cod_database_code               4307925