Approaching the limit of Cu(II)/Cu(I) mixed valency in a Cu(I)Br2-N-methylquinoxalinium hybrid compound.
Leblanc, Nicolas; Sproules, Stephen; Pasquier, Claude; Auban-Senzier, Pascale; Raffy, Helene; Powell, Annie K.; Chemical communications (Cambridge, England) 51 (2015) 12740–12743; doi:10.1039/c5cc04142b

data_7117580
_publ_section_title
;
 Approaching the limit of Cu(II)/Cu(I) mixed valency in a
 Cu(I)Br2-N-methylquinoxalinium hybrid compound.
;
_journal_issue                   64
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              12740
_journal_page_last               12743
_journal_paper_doi               10.1039/c5cc04142b
_journal_volume                  51
_journal_year                    2015
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C9 H9 N2, B F4'
_chemical_formula_sum            'C9 H9 B F4 N2'
_chemical_formula_weight         231.99
_chemical_name_common            (MQ)BF4
_chemical_name_systematic        'N-methylquinoxalinium tetrafluoroborate'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2014-02-21T14:10:13-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2015-05-12 deposited with the CCDC.
2015-06-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.232(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.372(2)
_cell_length_b                   6.2221(9)
_cell_length_c                   13.8278(19)
_cell_measurement_reflns_used    1470
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.32
_cell_measurement_theta_min      3.07
_cell_measurement_wavelength     0.71073
_cell_volume                     1065.0(3)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'image plate ( 34 cm diameter )'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_details      ' 130 frames, detector distance = 115 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.3 mm, multiple pinhole'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4693
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.398
_diffrn_reflns_theta_min         3.066
_diffrn_source                   'sealed X-ray tube, 12 x 0.4 mm fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.136
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             472
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeOH'
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.176
_exptl_crystal_size_min          0.102
_refine_diff_density_max         0.082
_refine_diff_density_min         -0.074
_refine_diff_density_rms         0.018
_refine_ls_extinction_coef       0.028(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.716
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     191
_refine_ls_number_reflns         2357
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.716
_refine_ls_R_factor_all          0.1415
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0423P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0992
_reflns_number_gt                707
_reflns_number_total             2357
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc04142b2.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        1064.9(3)
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               7117580