Crystal Structures and Vibrational Spectroscopy of [NBu4][Cu(CN)X] (X = Br, I) and [NBu4][Cu3(CN)4].CH3CN
Graham A. Bowmaker; Hans Hartl; Victoria Urban; Inorganic Chemistry 39 (2000) 4548–4554; doi:10.1021/ic000399s

data_4321409
_publ_contact_author
;
     Prof. Dr. Hans Hartl
     Institut f\"ur Chemie / Anorganische und Analytische Chemie
     Freie Universit\"at Berlin
     Fabeckstr. 34-36
     14195 Berlin
     Bundesrepublik Deutschland
;
_publ_contact_author_email       hartl@chemie.fu-berlin.de
_publ_contact_author_fax         '049 30 83852424'
_publ_contact_author_phone       '049 30 83854003'
_publ_section_title
;
 Crystal Structures and Vibrational Spectroscopy of [NBu4][Cu(CN)X] (X =
 Br, I) and [NBu4][Cu3(CN)4].CH3CN
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4548
_journal_page_last               4554
_journal_paper_doi               10.1021/ic000399s
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C34 H72 Br2 Cu2 N4'
_chemical_formula_weight         823.86
_chemical_name_systematic
;
 Tetra(n-butyl)ammonium bromo(cyano)cuprate(I)
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.4956(11)
_cell_length_b                   12.1741(8)
_cell_length_c                   19.2434(12)
_cell_measurement_reflns_used    4100
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      4.0
_cell_volume                     4098.7(5)
_computing_cell_refinement       'BRUKER SMART'
_computing_data_collection       'BRUKER SMART'
_computing_data_reduction        'BRUKER SHELXTL'
_computing_molecular_graphics    ORTEP32
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      143(2)
_diffrn_detector_area_resol_mean 'width 0.3 in omega'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'ccd area detector'
_diffrn_measurement_method       'phi and omega 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  0.0898
_diffrn_reflns_av_sigmaI/netI    0.0759
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            39470
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         1.98
_diffrn_standards_interval_time  20sec/frame
_exptl_absorpt_coefficient_mu    3.013
_exptl_absorpt_correction_T_max  0.83
_exptl_absorpt_correction_T_min  0.61
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS, Bruker AXS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'plate- and rodshaped'
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.822
_refine_diff_density_min         -1.285
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.076(9)
_refine_ls_extinction_coef       0.00000(8)
_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   0.922
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         9414
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.922
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          4.583
_refine_ls_shift/su_mean         0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0391P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0879
_reflns_number_gt                6546
_reflns_number_total             9414
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000399s_3.cif
_cod_data_source_block           newra33
_cod_database_code               4321409