Transition metal complexes of 2-amino-3,5-dihalopyridines: Syntheses, structures and magnetic properties of (3,5-diCAPH)2CuX4 and (3,5-diBAPH)2CuX4
Tremelling, Grant W.; Foxman, Bruce M.; Landee, Christopher P.; Turnbull, Mark M.; Willett, Roger D.; Dalton Transactions  (2009) 10518–10526; doi:10.1039/b914392k

data_7002940
_publ_section_title
;
 Transition metal complexes of 2-amino-3,5-dihalopyridines: Syntheses,
 structures and magnetic properties of (3,5-diCAPH)2CuX4 and
 (3,5-diBAPH)2CuX4
;
_journal_issue                   47
_journal_name_full               'Dalton Transactions'
_journal_page_first              10518
_journal_page_last               10526
_journal_paper_doi               10.1039/b914392k
_journal_year                    2009
_chemical_formula_sum            'C10 H10 Br8 Cu N4'
_chemical_formula_weight         889.04
_chemical_name_common
'bis(2-amino-3,5-dibromopyridinium) tetrabromocuprate'
_chemical_name_systematic
;
bis(2-amino-3,5-dibromopyridinium) tetrabromocuprate
;
_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                 107.096(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5870(11)
_cell_length_b                   11.5942(11)
_cell_length_c                   16.5555(15)
_cell_measurement_reflns_used    6808
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      29.68
_cell_measurement_theta_min      2.06
_cell_volume                     2125.8(3)
_computing_cell_refinement       'Bruker SAINT+ v. 6.36a'
_computing_data_collection       'Bruker SMART v. 5.626'
_computing_data_reduction        'Bruker SAINT+ v. 6.36a'
_computing_publication_material  'XCIF, Bruker SHELXTL v. 6.12'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      297(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker/Siemens SMART APEX'
_diffrn_measurement_method       '\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  0.0735
_diffrn_reflns_av_sigmaI/netI    0.0771
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12243
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        <0.01
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    16.065
_exptl_absorpt_correction_T_max  0.7394
_exptl_absorpt_correction_T_min  0.2487
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'via SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.778
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1628
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.908
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3746
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.908
_refine_ls_R_factor_all          0.0874
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0235P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0585
_refine_ls_wR_factor_ref         0.0703
_reflns_number_gt                2217
_reflns_number_total             3746
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b914392k.txt
_cod_data_source_block           bt253
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7002940