Mono-, di-, tetra- and heptanuclear copper(II) complexes with 4-(3,5-di-R-1H-pyrazol-1-yl)-6-methyl-2-(pyridin-2-yl)pyrimidines (R = H, Me): Syntheses, crystal structures and electrospray ionization mass spectrometry
Mark B. Bushuev; Yuri V. Gatilov; Elena B. Nikolaenkova; Vladimir G. Vasiliev; Viktor P. Krivopalov; Inorganica Chimica Acta 395 (2013) 95–103; doi:10.1016/j.ica.2012.10.018

data_1512896
_publ_section_title
;
 Mono-, di-, tetra- and heptanuclear copper(II) complexes with
 4-(3,5-di-R-1H-pyrazol-1-yl)-6-methyl-2-(pyridin-2-yl)pyrimidines (R = H,
 Me): Syntheses, crystal structures and electrospray ionization mass
 spectrometry
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              95
_journal_page_last               103
_journal_paper_doi               10.1016/j.ica.2012.10.018
_journal_volume                  395
_journal_year                    2013
_chemical_formula_moiety         'C52 H44 Cl12 Cu7 N20 2+, Cl6 Cu2 2-'
_chemical_formula_sum            'C52 H44 Cl18 Cu9 N20'
_chemical_formula_weight         2159.03
_chemical_name_systematic
; 
 dodekachloridotetrakis(4-(1H-pyrazol-1-yl)-2-(pyridin-2-yl)-6-
methylpyrimidine)heptacopper(2+) hexachloridodicuprate(2-)
;
_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
_cell_angle_alpha                65.086(11)
_cell_angle_beta                 82.287(11)
_cell_angle_gamma                87.008(15)
_cell_formula_units_Z            1
_cell_length_a                   9.743(5)
_cell_length_b                   13.755(6)
_cell_length_c                   15.437(8)
_cell_measurement_reflns_used    6914
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.78
_cell_measurement_theta_min      2.44
_cell_volume                     1859.3(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.887
_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  0.0470
_diffrn_reflns_av_sigmaI/netI    0.0648
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21720
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.81
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    3.219
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5661
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.928
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1063
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.384
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         9453
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+5.3772P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1130
_refine_ls_wR_factor_ref         0.1256
_reflns_number_gt                6824
_reflns_number_total             9453
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-395-95-103-3.cif
_cod_data_source_block           3_k177
_cod_original_sg_symbol_H-M      'P-1   '
_cod_database_code               1512896