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_4321407
_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            'C22 H39 Cu3 N6'
_chemical_formula_weight         578.21
_chemical_name_systematic
;
 Tetra(n-butyl)ammonium tetracyanotricuprate(I) acetronitrile solvate
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 113.30(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.8572(4)
_cell_length_b                   14.1180(3)
_cell_length_c                   13.39100(10)
_cell_measurement_reflns_used    1915
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     2927.0(7)
_computing_cell_refinement       'BRUKER SMART'
_computing_data_collection       'BRUKER SMART'
_computing_data_reduction        'BRUKER SHELXTL'
_computing_molecular_graphics    'ORTEP32 and DIAMOND2.1'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_detector_area_resol_mean 'width 0.3 in omega'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0366
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3117
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         1.66
_diffrn_standards_interval_time  20sec/frame
_exptl_absorpt_coefficient_mu    2.178
_exptl_absorpt_correction_T_max  0.7957
_exptl_absorpt_correction_T_min  0.5425
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS, Bruker AXS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         3117
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.272
_refine_ls_shift/su_mean         0.046
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0521P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0864
_refine_ls_wR_factor_ref         0.1016
_reflns_number_gt                2098
_reflns_number_total             3117
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000399s_1.cif
_cod_data_source_block           gbhh2
_cod_original_cell_volume        2927.11(10)
_cod_database_code               4321407