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#$Date: 2016-03-21 16:57:49 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178762 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/16/4101626.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_4101626
loop_
_publ_author_name
'Phillips, Anthony E.'
'Halder, Gregory J.'
'Chapman, Karena W.'
'Goodwin, Andrew L.'
'Kepert, Cameron J.'
_publ_contact_author
;
 Cameron J. Kepert
 School of Chemistry, F11
 University of Sydney
 NSW 2006
 Australia
;
_publ_contact_author_email       c.kepert@chem.usyd.edu.au
_publ_contact_author_fax         +61-2-9351-3329
_publ_contact_author_phone       +61-2-9351-5741
_publ_section_title
;
 Zero thermal expansion in a flexible, stable framework:
 tetramethylammonium copper(I) zinc(II) cyanide.
;
_journal_issue                   1
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10
_journal_page_last               11
_journal_paper_doi               10.1021/ja906895j
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C4 Cu N4 Zn, C4 H12 N'
_chemical_formula_sum            'C8 H12 Cu N5 Zn'
_chemical_formula_weight         307.14
_chemical_name_common
; 
 tetramethylammonium copper(I) zinc cyanide
;
_chemical_name_systematic
; 
 tetramethylammonium copper(I) zinc cyanide
;
_space_group_IT_number           198
_symmetry_cell_setting           cubic
_symmetry_Int_Tables_number      198
_symmetry_space_group_name_Hall  'P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P 21 3'
_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                   11.6012(3)
_cell_length_b                   11.6012(3)
_cell_length_c                   11.6012(3)
_cell_measurement_reflns_used    2981
_cell_measurement_temperature    105(2)
_cell_measurement_theta_max      53.779
_cell_measurement_theta_min      4.966
_cell_volume                     1561.38(7)
_computing_cell_refinement       'SMART (BrukerAXS, 1997)'
_computing_data_collection       'SMART (BrukerAXS, 1997)'
_computing_data_reduction        'SAINT+ (BrukerAXS, 1997)'
_computing_molecular_graphics    'Mercury 1.4.1'
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       ω
_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    0.0199
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            1091
_diffrn_reflns_theta_full        26.35
_diffrn_reflns_theta_max         26.35
_diffrn_reflns_theta_min         1.76
_diffrn_standards_decay_%        0.00
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.879
_exptl_absorpt_correction_T_max  0.708
_exptl_absorpt_correction_T_min  0.546
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker 1997'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.235
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     49
_refine_ls_number_reflns         1084
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.235
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0222
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0112P)²+0.6222P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0525
_refine_ls_wR_factor_ref         0.0533
_reflns_number_gt                1057
_reflns_number_total             1084
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ja906895j_si_002.cif
_cod_data_source_block           100K
_cod_original_sg_symbol_H-M      P213
_cod_database_code               4101626
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
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
C1 C 0.4162(5) 0.5838(5) 0.0838(5) 0.056(3) Uani 1 3 d S . .
N2 N 0.1497(4) 0.6431(4) 0.3214(3) 0.0470(9) Uani 1 1 d . . .
C2 C 0.4131(4) 0.4050(4) -0.1212(4) 0.0413(10) Uani 1 1 d . . .
Cu1 Cu 0.51310(5) 0.48690(5) -0.01310(5) 0.0381(3) Uani 1 3 d S . .
Zn2 Zn 0.26113(5) 0.73887(5) 0.23887(5) 0.0334(2) Uani 1 3 d S . .
N1 N 0.3587(5) 0.6413(5) 0.1413(5) 0.055(2) Uani 1 3 d S . .
N100 N 0.2449(2) 0.7449(2) 0.7551(2) 0.0472(11) Uani 1 3 d S . .
C101 C 0.1714(4) 0.6714(4) 0.8286(4) 0.084(3) Uani 1 3 d S . .
H10A H 0.2195 0.6150 0.8691 0.125 Uiso 0.3333 1 calc PR . .
H10B H 0.1150 0.6309 0.7805 0.125 Uiso 0.3333 1 calc PR . .
H10C H 0.1309 0.7195 0.8850 0.125 Uiso 0.3333 1 calc PR . .
C102 C 0.3355(7) 0.7980(9) 0.8230(6) 0.208(6) Uani 1 1 d . . .
H10D H 0.3012 0.8405 0.8874 0.312 Uiso 1 1 calc R . .
H10E H 0.3796 0.8512 0.7744 0.312 Uiso 1 1 calc R . .
H10F H 0.3869 0.7381 0.8530 0.312 Uiso 1 1 calc R . .
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
C1 0.056(3) 0.056(3) 0.056(3) -0.009(3) 0.009(3) 0.009(3)
N2 0.043(2) 0.051(2) 0.046(2) 0.0036(18) 0.0038(17) -0.0063(18)
C2 0.036(2) 0.045(3) 0.043(2) 0.0059(19) 0.0070(19) 0.003(2)
Cu1 0.0381(3) 0.0381(3) 0.0381(3) -0.0041(2) 0.0041(2) 0.0041(2)
Zn2 0.0334(2) 0.0334(2) 0.0334(2) -0.0028(2) 0.0028(2) 0.0028(2)
N1 0.055(2) 0.055(2) 0.055(2) -0.011(2) 0.011(2) 0.011(2)
N100 0.0472(11) 0.0472(11) 0.0472(11) 0.0050(17) 0.0050(17) -0.0050(17)
C101 0.084(3) 0.084(3) 0.084(3) 0.020(2) 0.020(2) -0.020(2)
C102 0.155(7) 0.376(15) 0.093(5) 0.012(7) -0.016(5) -0.187(9)
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'
H H 0.0000 0.0000 '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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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
_geom_angle_publ_flag
N1 C1 Cu1 180.0(11) . . ?
C2 N2 Zn2 172.9(3) 2_565 . ?
N2 C2 Cu1 175.8(3) 2_564 . ?
C1 Cu1 C2 107.96(14) . 7_564 ?
C1 Cu1 C2 107.96(14) . . ?
C2 Cu1 C2 110.94(13) 7_564 . ?
C1 Cu1 C2 107.96(14) . 10_655 ?
C2 Cu1 C2 110.94(13) 7_564 10_655 ?
C2 Cu1 C2 110.94(13) . 10_655 ?
N2 Zn2 N2 109.28(13) 10_655 . ?
N2 Zn2 N2 109.28(13) 10_655 7_564 ?
N2 Zn2 N2 109.28(13) . 7_564 ?
N2 Zn2 N1 109.66(13) 10_655 . ?
N2 Zn2 N1 109.66(13) . . ?
N2 Zn2 N1 109.66(13) 7_564 . ?
C1 N1 Zn2 180.0(10) . . ?
C102 N100 C102 108.5(3) . 8_656 ?
C102 N100 C102 108.5(3) . 11_466 ?
C102 N100 C102 108.5(3) 8_656 11_466 ?
C102 N100 C101 110.5(3) . . ?
C102 N100 C101 110.5(3) 8_656 . ?
C102 N100 C101 110.5(3) 11_466 . ?
N100 C101 H10A 109.5 . . ?
N100 C101 H10B 109.5 . . ?
H10A C101 H10B 109.5 . . ?
N100 C101 H10C 109.5 . . ?
H10A C101 H10C 109.5 . . ?
H10B C101 H10C 109.5 . . ?
N100 C102 H10D 109.5 . . ?
N100 C102 H10E 109.5 . . ?
H10D C102 H10E 109.5 . . ?
N100 C102 H10F 109.5 . . ?
H10D C102 H10F 109.5 . . ?
H10E C102 H10F 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.155(13) . ?
C1 Cu1 1.947(10) . ?
N2 C2 1.134(6) 2_565 ?
N2 Zn2 1.955(4) . ?
C2 N2 1.134(6) 2_564 ?
C2 Cu1 1.955(5) . ?
Cu1 C2 1.955(5) 7_564 ?
Cu1 C2 1.955(5) 10_655 ?
Zn2 N2 1.955(4) 10_655 ?
Zn2 N2 1.955(4) 7_564 ?
Zn2 N1 1.961(9) . ?
N100 C102 1.451(6) . ?
N100 C102 1.451(6) 8_656 ?
N100 C102 1.451(6) 11_466 ?
N100 C101 1.478(8) . ?
C101 H10A 0.9800 . ?
C101 H10B 0.9800 . ?
C101 H10C 0.9800 . ?
C102 H10D 0.9800 . ?
C102 H10E 0.9800 . ?
C102 H10F 0.9800 . ?
