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_1512895
_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         'C13 H11 Cl2 Cu N5'
_chemical_formula_sum            'C13 H11 Cl2 Cu N5'
_chemical_formula_weight         371.71
_chemical_name_systematic
; 
 dichlorido(4-(1H-pyrazol-1-yl)-2-(pyridin-2-yl)-6-methylpyrimidine)copper 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 92.914(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.233(2)
_cell_length_b                   9.310(3)
_cell_length_c                   16.356(5)
_cell_measurement_reflns_used    927
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.06
_cell_measurement_theta_min      3.11
_cell_volume                     1404.1(7)
_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 0.970
_diffrn_measured_fraction_theta_max 0.962
_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  0.0819
_diffrn_reflns_av_sigmaI/netI    0.1234
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4048
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.27
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    1.934
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.3957
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.758
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.702
_refine_diff_density_min         -1.129
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         2447
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1030
_refine_ls_R_factor_gt           0.0541
_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^)+(0.0356P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1065
_refine_ls_wR_factor_ref         0.1176
_reflns_number_gt                1446
_reflns_number_total             2447
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-395-95-103-2.cif
_cod_data_source_block           2_k176
_cod_original_cell_volume        1404.3(7)
_cod_original_sg_symbol_H-M      'P2(1)/c  '
_cod_database_code               1512895