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#$Date: 2016-03-23 00:41:36 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179123 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/85/4308589.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4308589
loop_
_publ_author_name
'Torsten Küppers'
'Eduard Bernhardt'
'Helge Willner'
'Henning W. Rohm'
'Martin Köckerling'
_publ_contact_author
;
Martin Köckerling
Universität Rostock
Fachbereich Chemie
Anorganische Chemie/Festkörperchemie
Albert-Einstein-Str. 3a
D-18057 Rostock
Germany
;
_publ_contact_author_email       martin.koeckerling@chemie.uni-rostock.de
_publ_contact_author_fax         intl-code-(0)381-498-6382
_publ_contact_author_phone       intl-code-(0)381-498-6390
_publ_section_title
;
Tetracyanoborate Salts M[B(CN)4] with M = Singly Charged Cations:
Properties and Structures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1015
_journal_page_last               1022
_journal_paper_doi               10.1021/ic048780q
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C4 B N4 Rb'
_chemical_formula_structural     'Rb B (CN)4'
_chemical_formula_sum            'C4 B N4 Rb'
_chemical_formula_weight         200.36
_chemical_name_systematic        Rubidium-tetracyanoborate
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             august-2-2004
_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                   7.1354(2)
_cell_length_b                   7.1354(2)
_cell_length_c                   14.8197(6)
_cell_measurement_reflns_used    1885
_cell_measurement_temperature    566(2)
_cell_measurement_theta_max      32.25
_cell_measurement_theta_min      3.17
_cell_volume                     754.53(4)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.894
_diffrn_measured_fraction_theta_max 0.894
_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  0.0258
_diffrn_reflns_av_sigmaI/netI    0.0257
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            2797
_diffrn_reflns_theta_full        36.28
_diffrn_reflns_theta_max         36.28
_diffrn_reflns_theta_min         3.17
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    6.484
_exptl_absorpt_correction_T_max  0.6596
_exptl_absorpt_correction_T_min  0.2099
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, Bruker, 2000)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.764
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.57
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.291
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       0.051(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_matrix_type           full
_refine_ls_number_parameters     24
_refine_ls_number_reflns         818
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0250
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0169P)²+0.4438P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0476
_refine_ls_wR_factor_ref         0.0523
_reflns_number_gt                645
_reflns_number_total             818
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048780qsi20041119_090312_8.cif
_cod_data_source_block           RbB(CN)4
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4308589
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
B1 B 0.0000 0.2500 0.1250 0.0260(5) Uani 1 4 d S . .
C1 C 0.1505(2) 0.3550(2) 0.06409(10) 0.0311(3) Uani 1 1 d . . .
N1 N 0.2596(2) 0.4320(2) 0.02230(11) 0.0465(3) Uani 1 1 d . . .
Rb1 Rb 0.5000 0.7500 0.1250 0.03463(13) Uani 1 4 d S . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
B1 0.0256(7) 0.0256(7) 0.0268(13) 0.000 0.000 0.000
C1 0.0314(7) 0.0288(6) 0.0333(7) -0.0009(5) 0.0013(5) 0.0001(5)
N1 0.0458(8) 0.0432(8) 0.0504(8) 0.0011(7) 0.0118(7) -0.0060(6)
Rb1 0.03555(14) 0.03555(14) 0.03281(17) 0.000 0.000 0.000
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C1 B1 C1 110.84(10) 12_666 15
C1 B1 C1 108.79(5) 12_666 6_454
C1 B1 C1 108.79(5) 15 6_454
C1 B1 C1 108.79(5) 12_666 .
C1 B1 C1 108.79(5) 15 .
C1 B1 C1 110.84(10) 6_454 .
N1 C1 B1 178.42(15) . .
C1 N1 Rb1 124.51(12) . 9_665
C1 N1 Rb1 116.56(12) . .
Rb1 N1 Rb1 109.66(4) 9_665 .
N1 Rb1 N1 89.16(6) 8_454 3
N1 Rb1 N1 120.48(4) 8_454 14
N1 Rb1 N1 120.48(4) 3 14
N1 Rb1 N1 120.48(4) 8_454 9_665
N1 Rb1 N1 120.48(4) 3 9_665
N1 Rb1 N1 89.16(6) 14 9_665
N1 Rb1 N1 162.73(6) 8_454 .
N1 Rb1 N1 73.57(2) 3 .
N1 Rb1 N1 70.39(2) 14 .
N1 Rb1 N1 70.34(4) 9_665 .
N1 Rb1 N1 70.34(4) 8_454 12_766
N1 Rb1 N1 70.39(2) 3 12_766
N1 Rb1 N1 162.73(6) 14 12_766
N1 Rb1 N1 73.57(2) 9_665 12_766
N1 Rb1 N1 102.86(2) . 12_766
N1 Rb1 N1 70.39(2) 8_454 15_565
N1 Rb1 N1 70.34(4) 3 15_565
N1 Rb1 N1 73.57(2) 14 15_565
N1 Rb1 N1 162.73(6) 9_665 15_565
N1 Rb1 N1 102.86(2) . 15_565
N1 Rb1 N1 123.70(6) 12_766 15_565
N1 Rb1 N1 73.57(2) 8_454 6_564
N1 Rb1 N1 162.73(6) 3 6_564
N1 Rb1 N1 70.34(4) 14 6_564
N1 Rb1 N1 70.39(2) 9_665 6_564
N1 Rb1 N1 123.70(6) . 6_564
N1 Rb1 N1 102.86(2) 12_766 6_564
N1 Rb1 N1 102.86(2) 15_565 6_564
N1 Rb1 Rb1 36.20(3) 8_454 13_665
N1 Rb1 Rb1 77.34(3) 3 13_665
N1 Rb1 Rb1 154.32(3) 14 13_665
N1 Rb1 Rb1 97.17(3) 9_665 13_665
N1 Rb1 Rb1 135.12(3) . 13_665
N1 Rb1 Rb1 34.13(3) 12_766 13_665
N1 Rb1 Rb1 98.51(3) 15_565 13_665
N1 Rb1 Rb1 88.34(3) 6_564 13_665
N1 Rb1 Rb1 154.32(3) 8_454 9_665
N1 Rb1 Rb1 97.17(3) 3 9_665
N1 Rb1 Rb1 77.34(3) 14 9_665
N1 Rb1 Rb1 36.20(3) 9_665 9_665
N1 Rb1 Rb1 34.13(3) . 9_665
N1 Rb1 Rb1 88.34(3) 12_766 9_665
N1 Rb1 Rb1 135.12(3) 15_565 9_665
N1 Rb1 Rb1 98.51(3) 6_564 9_665
Rb1 Rb1 Rb1 121.256(2) 13_665 9_665
N1 Rb1 Rb1 77.34(3) 8_454 13_565
N1 Rb1 Rb1 36.20(3) 3 13_565
N1 Rb1 Rb1 97.17(3) 14 13_565
N1 Rb1 Rb1 154.32(3) 9_665 13_565
N1 Rb1 Rb1 88.34(3) . 13_565
N1 Rb1 Rb1 98.51(3) 12_766 13_565
N1 Rb1 Rb1 34.13(3) 15_565 13_565
N1 Rb1 Rb1 135.12(3) 6_564 13_565
Rb1 Rb1 Rb1 87.838(3) 13_665 13_565
Rb1 Rb1 Rb1 121.256(2) 9_665 13_565
N1 Rb1 Rb1 97.17(3) 8_454 9_675
N1 Rb1 Rb1 154.32(3) 3 9_675
N1 Rb1 Rb1 36.20(3) 14 9_675
N1 Rb1 Rb1 77.34(3) 9_665 9_675
N1 Rb1 Rb1 98.51(3) . 9_675
N1 Rb1 Rb1 135.12(3) 12_766 9_675
N1 Rb1 Rb1 88.34(3) 15_565 9_675
N1 Rb1 Rb1 34.13(3) 6_564 9_675
Rb1 Rb1 Rb1 121.256(2) 13_665 9_675
Rb1 Rb1 Rb1 87.838(3) 9_665 9_675
Rb1 Rb1 Rb1 121.256(2) 13_565 9_675
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
B1 C1 1.5904(14) 12_666
B1 C1 1.5904(14) 15
B1 C1 1.5904(14) 6_454
B1 C1 1.5904(14) .
C1 N1 1.136(2) .
N1 Rb1 3.0648(14) 9_665
N1 Rb1 3.2261(15) .
Rb1 N1 3.0648(14) 8_454
Rb1 N1 3.0648(14) 3
Rb1 N1 3.0648(14) 14
Rb1 N1 3.0648(14) 9_665
Rb1 N1 3.2261(15) 12_766
Rb1 N1 3.2261(15) 15_565
Rb1 N1 3.2261(15) 6_564
Rb1 Rb1 5.14344(13) 13_665
Rb1 Rb1 5.14344(13) 9_665
Rb1 Rb1 5.14344(13) 13_565
Rb1 Rb1 5.14344(13) 9_675
