Polynuclear copper(ii) pyrazolate complexes: temperature-dependent protonolysis reactions, crystal structures and high catalytic activity toward the condensation of nitriles with 2-aminoalcohol.
Wang, Ling; Guo, Bin; Li, Hong-Xi; Li, Qi; Li, Hai-Yan; Lang, Jian-Ping; Dalton transactions (Cambridge, England : 2003) 42 (2013) 15570–15580; doi:10.1039/c3dt51970h

data_7023754
_publ_section_title
;
 Polynuclear copper(ii) pyrazolate complexes: temperature-dependent
 protonolysis reactions, crystal structures and high catalytic activity
 toward the condensation of nitriles with 2-aminoalcohol.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15570
_journal_page_last               15580
_journal_paper_doi               10.1039/c3dt51970h
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C48 H60 Cu6 N12 O30'
_chemical_formula_sum            'C48 H60 Cu6 N12 O30'
_chemical_formula_weight         1666.32
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                95.39(3)
_cell_angle_beta                 115.01(3)
_cell_angle_gamma                114.83(3)
_cell_formula_units_Z            2
_cell_length_a                   15.722(3)
_cell_length_b                   16.304(3)
_cell_length_c                   16.721(3)
_cell_measurement_reflns_used    9659
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      31.48
_cell_measurement_theta_min      2.35
_cell_volume                     3328(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0196
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            184702
_diffrn_reflns_theta_full        31.58
_diffrn_reflns_theta_max         31.58
_diffrn_reflns_theta_min         2.34
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.976
_exptl_absorpt_correction_T_max  0.5447
_exptl_absorpt_correction_T_min  0.5205
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1692
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.35
_refine_diff_density_max         1.010
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     883
_refine_ls_number_reflns         22193
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0312
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0445P)^2^+1.3303P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0772
_refine_ls_wR_factor_ref         0.0845
_reflns_number_gt                18161
_reflns_number_total             22193
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51970h.txt
_cod_data_source_block           2
_cod_original_cell_volume        3327.6(11)
_cod_database_code               7023754