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#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/71/2227116.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2227116
loop_
_publ_author_name
'Chatterjee, Sayandev'
'Del Negro, Andrew S.'
'Edwards, Matthew K.'
'Twamley, Brendan'
'Krause, Jeanette A.'
'Bryan, Samuel A.'
_publ_section_title
;
 trans-K₃[TcO₂(CN)₄]
;
_journal_coeditor_code           WM2375
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i61
_journal_page_last               i62
_journal_paper_doi               10.1107/S1600536810028205
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'K 3 [Tc O2 (C N)4]'
_chemical_formula_moiety         '3K, C4 N4 O2 Tc'
_chemical_formula_structural     'K 3 [Tc O2 (C N)4]'
_chemical_formula_sum            'C4 K3 N4 O2 Tc'
_chemical_formula_weight         351.38
_chemical_name_systematic
;
tripotassium trans-tetracyanidodioxidotechnetate(V)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                108.3050(10)
_cell_angle_beta                 109.816(2)
_cell_angle_gamma                104.1430(10)
_cell_formula_units_Z            1
_cell_length_a                   6.2539(6)
_cell_length_b                   6.9389(6)
_cell_length_c                   7.4347(7)
_cell_measurement_reflns_used    3550
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      3.23
_cell_volume                     265.01(4)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'SMART (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_molecular_graphics
'SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2010)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0724
_diffrn_reflns_av_sigmaI/netI    0.0501
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3949
_diffrn_reflns_theta_full        26.48
_diffrn_reflns_theta_max         26.48
_diffrn_reflns_theta_min         3.23
_exptl_absorpt_coefficient_mu    2.513
_exptl_absorpt_correction_T_max  0.705
_exptl_absorpt_correction_T_min  0.490
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.202
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             168
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.774
_refine_diff_density_min         -0.900
_refine_ls_extinction_coef       0.024(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXTL (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_matrix_type           full
_refine_ls_number_parameters     68
_refine_ls_number_reflns         1097
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0204
_refine_ls_R_factor_gt           0.0199
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0114P)²+0.0622P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0484
_refine_ls_wR_factor_ref         0.0487
_reflns_number_gt                1064
_reflns_number_total             1097
_reflns_threshold_expression     >σ(I)
_cod_data_source_file            wm2375.cif
_cod_data_source_block           I
_cod_database_code               2227116
_cod_database_fobs_code          2227116
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
K K1 0.5000 0.0000 1.0000 0.01358(15) Uani d S 1 . .
K K2 0.04367(6) 0.33536(7) 0.69923(6) 0.01283(13) Uani d . 1 . .
Tc Tc1 0.5000 0.5000 0.5000 0.00885(11) Uani d S 1 . .
O O1 0.6628(2) 0.3641(2) 0.39016(18) 0.0123(3) Uani d . 1 . .
N N1 0.6522(3) 0.3389(3) 0.8804(2) 0.0159(4) Uani d . 1 . .
N N2 -0.0098(3) 0.0509(3) 0.2506(2) 0.0161(4) Uani d . 1 . .
C C1 0.5999(3) 0.3996(3) 0.7507(3) 0.0120(4) Uani d . 1 . .
C C2 0.1707(3) 0.2034(3) 0.3254(3) 0.0123(4) Uani d . 1 . .
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'
K K 0.2009 0.2494 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tc Tc -1.4390 0.7593 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Tc1 O1 2_666 . 180.0 ?
O1 Tc1 C1 2_666 2_666 90.13(6) ?
O1 Tc1 C1 . 2_666 89.87(6) ?
O1 Tc1 C1 2_666 . 89.87(6) ?
O1 Tc1 C1 . . 90.13(6) ?
C1 Tc1 C1 2_666 . 179.9990(10) ?
O1 Tc1 C2 2_666 . 88.60(6) ?
O1 Tc1 C2 . . 91.40(6) ?
C1 Tc1 C2 2_666 . 92.34(7) ?
C1 Tc1 C2 . . 87.66(7) ?
O1 Tc1 C2 2_666 2_666 91.40(6) ?
O1 Tc1 C2 . 2_666 88.60(6) ?
C1 Tc1 C2 2_666 2_666 87.66(7) ?
C1 Tc1 C2 . 2_666 92.34(7) ?
C2 Tc1 C2 . 2_666 180.0 ?
Tc1 O1 K2 . 1_655 111.70(5) ?
Tc1 O1 K1 . 1_554 131.58(5) ?
K2 O1 K1 1_655 1_554 107.62(4) ?
Tc1 O1 K2 . 2_666 106.54(6) ?
K2 O1 K2 1_655 2_666 98.26(4) ?
K1 O1 K2 1_554 2_666 94.38(4) ?
N1 C1 Tc1 . . 177.71(16) y
N2 C2 Tc1 . . 172.74(15) y
C1 N1 K2 . 2_667 116.78(14) ?
C1 N1 K1 . . 145.03(14) ?
K2 N1 K1 2_667 . 94.44(5) ?
C1 N1 K2 . 1_655 73.15(11) ?
K2 N1 K2 2_667 1_655 100.94(5) ?
K1 N1 K2 . 1_655 118.11(6) ?
C2 N2 K2 . 2_556 124.85(13) ?
C2 N2 K1 . 1_454 127.59(15) ?
K2 N2 K1 2_556 1_454 107.51(6) ?
O1 K1 O1 2_656 1_556 180.00(5) ?
O1 K1 N1 2_656 . 97.86(4) ?
O1 K1 N1 1_556 . 82.14(4) ?
O1 K1 N1 2_656 2_657 82.14(4) ?
O1 K1 N1 1_556 2_657 97.86(4) ?
N1 K1 N1 . 2_657 180.00(7) ?
O1 K1 N2 2_656 1_656 104.18(4) ?
O1 K1 N2 1_556 1_656 75.82(4) ?
N1 K1 N2 . 1_656 95.00(5) ?
N1 K1 N2 2_657 1_656 85.00(5) ?
O1 K1 N2 2_656 2_556 75.82(4) ?
O1 K1 N2 1_556 2_556 104.18(4) ?
N1 K1 N2 . 2_556 85.00(5) ?
N1 K1 N2 2_657 2_556 95.00(5) ?
N2 K1 N2 1_656 2_556 180.0 ?
N2 K2 O1 2_556 1_455 123.16(4) ?
N2 K2 N1 2_556 2_667 101.64(5) ?
O1 K2 N1 1_455 2_667 125.77(5) ?
N2 K2 O1 2_556 2_666 139.59(4) ?
O1 K2 O1 1_455 2_666 81.74(4) ?
N1 K2 O1 2_667 2_666 82.38(5) ?
N2 K2 N1 2_556 1_455 84.21(5) ?
O1 K2 N1 1_455 1_455 77.02(4) ?
N1 K2 N1 2_667 1_455 79.06(5) ?
O1 K2 N1 2_666 1_455 135.31(4) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Tc1 O1 2_666 1.7721(12) ?
Tc1 O1 . 1.7721(12) y
Tc1 C1 2_666 2.1423(19) ?
Tc1 C1 . 2.1423(19) y
Tc1 C2 . 2.145(2) y
Tc1 C2 2_666 2.145(2) ?
O1 K2 1_655 2.7937(12) ?
O1 K1 1_554 2.8235(13) ?
O1 K2 2_666 2.8262(14) ?
N1 C1 . 1.150(3) y
N1 K2 2_667 2.8152(16) ?
N1 K2 1_655 3.1710(16) ?
N2 C2 . 1.151(3) y
N2 K2 2_556 2.7876(19) ?
N2 K1 1_454 2.8598(15) ?
K1 O1 2_656 2.8235(13) ?
K1 O1 1_556 2.8235(13) ?
K1 N1 . 2.8315(18) ?
K1 N1 2_657 2.8315(18) ?
K1 N2 1_656 2.8598(15) ?
K1 N2 2_556 2.8598(15) ?
K2 N2 2_556 2.7877(19) ?
K2 O1 1_455 2.7936(12) ?
K2 N1 2_667 2.8152(16) ?
K2 O1 2_666 2.8262(14) ?
K2 N1 1_455 3.1710(16) ?
