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_4321408
_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 Cu2 I2 N4'
_chemical_formula_weight         917.84
_chemical_name_systematic
;
 Tetra(n-butyl)ammonium iodo(cyano)cuprate(I)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 111.710(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.683(2)
_cell_length_b                   12.233(2)
_cell_length_c                   17.632(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.00
_cell_measurement_theta_min      2.49
_cell_volume                     4345.1(11)
_computing_cell_refinement       'ENRAF-NONIUS CAD4'
_computing_data_collection       'ENRAF-NONIUS CAD4'
_computing_data_reduction        'MOLEN DELFT INSTRUMENTS'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.925
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       OMEGA-THETA-SCAN
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7121
_diffrn_reflns_theta_full        23.00
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         2.49
_exptl_absorpt_coefficient_mu    2.424
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle-sharped
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.045
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         5596
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.282
_refine_ls_shift/su_mean         0.019
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+3.0276P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0904
_reflns_number_gt                3951
_reflns_number_total             5596
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000399s_2.cif
_cod_data_source_block           new2t
_cod_database_code               4321408