Nine compounds containing high-nuclearity [Cu~<i>n~</i><i>X</i>~2<i>n~+2</i>]^2{-^} (<i>n</i> = 4, 5 or 7; <i>X</i> = Cl or Br) quasi-planar oligomers
Kelley, Annette; Akkina, Subhash; Devarapally, Goutham K.; Nalla, Soujanya; Pasam, Divya; Madhabushi, Shravani; Bond, Marcus R.; Acta Crystallographica Section C 67 (2011) m22–m34; doi:10.1107/S0108270110049024

data_2017969
_publ_section_title
;
 Nine compounds containing high-nuclearity
 [Cu~<i>n~</i><i>X</i>~2<i>n~+2</i>]^2{-^} (<i>n</i> = 4, 5 or 7;
 <i>X</i> = Cl or Br) quasi-planar oligomers
;
_journal_coeditor_code           SK3391
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m22
_journal_page_last               m34
_journal_paper_doi               10.1107/S0108270110049024
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '(C7 H10 N)2 [Cu4 Br10]'
_chemical_formula_moiety         '2(C7 H10 N1 +), Br10 Cu4 2-'
_chemical_formula_sum            'C14 H20 Br10 Cu4 N2'
_chemical_formula_weight         1269.549
_chemical_name_systematic
;
bis(2,3-dimethylpyridinium) hexa-\m-chlorido-tetrachloridotetracuprate(II)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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
_cell_angle_alpha                90
_cell_angle_beta                 96.459(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.7548(5)
_cell_length_b                   12.5783(8)
_cell_length_c                   12.2179(5)
_cell_measurement_reflns_used    3960
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      29.131
_cell_measurement_theta_min      2.91
_cell_volume                     1489.61(14)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 1997) and ORTEPIII (Burnett & Johnson,
1996)
;
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>, 1993)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0744
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7293
_diffrn_reflns_reduction_process
;
 Scaled and merged with Sortav
 R. H. Blessing (1987), Cryst. Rev. 1, 3--58.
 R. H. Blessing (1989), J. Appl. Cryst. 22, 396--397.
;
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         29.11
_diffrn_reflns_theta_min         4.09
_exptl_absorpt_coefficient_mu    16.237
_exptl_absorpt_correction_T_max  0.197
_exptl_absorpt_correction_T_min  0.093
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO/SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    2.831
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.785
_refine_diff_density_min         -0.927
_refine_ls_extinction_coef       0.0084(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         3901
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1223
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0423P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.1131
_reflns_number_gt                2141
_reflns_number_total             3901
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3391.cif
_cod_data_source_block           IV
_cod_database_code               2017969
_cod_database_fobs_code          2017969