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_4329875
_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         'C16 H22 Cu I N6, C2 H3 N'
_chemical_formula_sum            'C18 H25 Cu I N7'
_chemical_formula_weight         529.89
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 103.9990(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2452(6)
_cell_length_b                   8.1570(4)
_cell_length_c                   20.5917(9)
_cell_measurement_reflns_used    9862
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.54
_cell_measurement_theta_min      2.70
_cell_volume                     2158.67(17)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0268
_diffrn_reflns_av_sigmaI/netI    0.0155
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            50306
_diffrn_reflns_theta_full        30.55
_diffrn_reflns_theta_max         30.55
_diffrn_reflns_theta_min         1.66
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.459
_exptl_absorpt_correction_T_max  0.7087
_exptl_absorpt_correction_T_min  0.5961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
program SADABS, Bruker (2001).
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_description       plate
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.731
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         6602
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0229
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0247P)^2^+1.1670P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0551
_refine_ls_wR_factor_ref         0.0578
_reflns_number_gt                5682
_reflns_number_total             6602
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300843a_si_002_3.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4329875