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_4307927
_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         'C50 H70 Cu4 N26 O8 4+, 4(N O3 -), 5(H2 O)'
_chemical_formula_sum            'C50 H80 Cu4 N30 O25'
_chemical_formula_weight         1755.60
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.003(5)
_cell_angle_beta                 106.635(5)
_cell_angle_gamma                93.850(5)
_cell_formula_units_Z            1
_cell_length_a                   9.5728(6)
_cell_length_b                   13.1348(8)
_cell_length_c                   14.5660(9)
_cell_measurement_reflns_used    27830
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      24.74
_cell_measurement_theta_min      1.56
_cell_volume                     1743.26(19)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0554
_diffrn_reflns_av_sigmaI/netI    0.0321
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            27830
_diffrn_reflns_theta_full        24.74
_diffrn_reflns_theta_max         24.74
_diffrn_reflns_theta_min         1.56
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.305
_exptl_absorpt_correction_T_max  0.7711
_exptl_absorpt_correction_T_min  0.5865
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2002)'
_exptl_crystal_colour            'blue green'
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             906
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         5954
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0312
_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^)+(0.0491P)^2^+1.3486P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0860
_reflns_number_gt                5232
_reflns_number_total             5954
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062434msi20061219_032313_4.cif
_cod_data_source_block           2
_cod_database_code               4307927