Copper(I) Complexes with Trispyrazolylmethane Ligands: Synthesis, Characterization, and Catalytic Activity in Cross-Coupling Reactions
Estela Haldón; Eleuterio Álvarez; M. Carmen Nicasio; Pedro J. Pérez; Inorganic Chemistry 51 (2012) 8298–8306; doi:10.1021/ic300843a

data_4329873
_publ_contact_author_address
;
    Laboratorio de Cat\'alisis Homog\'enea, Departamento de Qu\'imica y
    Ciencias de los Materiales, Unidad Asociada al CSIC, Centro de
    Investigaci\'on en Qu\'imica Sostenible (CIQSO), Campus de El Carmen s/n,
    Universidad de Huelva, 21007-Huelva, Spain
;
_publ_contact_author_email       perez@dqcm.uhu.es
_publ_contact_author_name        'Prof. Pedro J. P\'erez'
_publ_contact_author_phone       '+34 959219956'
_publ_section_title
;
 Copper(I) Complexes with Trispyrazolylmethane Ligands: Synthesis,
 Characterization, and Catalytic Activity in Cross-Coupling Reactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8298
_journal_page_last               8306
_journal_paper_doi               10.1021/ic300843a
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         '2(C39 H43 Cu N7), Cu2 I4, 3(C2 H3 N)'
_chemical_formula_sum            'C84 H95 Cu4 I4 N17'
_chemical_formula_weight         2104.53
_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                67.6770(10)
_cell_angle_beta                 71.0740(10)
_cell_angle_gamma                89.7950(10)
_cell_formula_units_Z            1
_cell_length_a                   11.9747(5)
_cell_length_b                   14.0027(6)
_cell_length_c                   15.1715(6)
_cell_measurement_reflns_used    9866
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.83
_cell_measurement_theta_min      2.23
_cell_volume                     2205.16(16)
_computing_cell_refinement       'APEX2 Software Suite (Bruker, 2007)'
_computing_data_collection       'APEX2 Software Suite (Bruker, 2007)'
_computing_data_reduction        'APEX2 Software Suite (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL and publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2002 (Burla et al., 2003)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type
;
 Bruker-Nonius X8kappa APEX II CCD area detector
;
_diffrn_measurement_method       'phi and omega scans with narrow frames'
_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  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0195
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            75807
_diffrn_reflns_theta_full        30.66
_diffrn_reflns_theta_max         30.66
_diffrn_reflns_theta_min         1.55
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.403
_exptl_absorpt_correction_T_max  0.7951
_exptl_absorpt_correction_T_min  0.6323
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS, Bruker (2006). APEX 2. Version 2.1. Bruker Analytical
 x-ray Solutions, Madison, Wisconsin, USA.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_description       prism
_exptl_crystal_F_000             1046
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.315
_refine_diff_density_min         -1.219
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         13472
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0344
_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^)+(0.0390P)^2^+2.2261P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.0911
_reflns_number_gt                10698
_reflns_number_total             13472
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300843a_si_002_1.cif
_cod_data_source_block           3
_cod_database_code               4329873