#------------------------------------------------------------------------------
#$Date: 2019-11-23 20:31:29 +0200 (Sat, 23 Nov 2019) $
#$Revision: 234869 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/95/4349541.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_4349541
loop_
_publ_author_name
'Shi, Chao'
'Han, Xiang-Bin'
'Wang, Ya'
'Zhang, Wen'
_publ_section_title
;
 Tuning dielectric transitions by B′-site mixing in hybrid double
 perovskite crystals (CH3NH3)2[K1−xRbxCo(CN)6] (x = 0.23--0.62)
;
_journal_issue                   12
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              1604
_journal_paper_doi               10.1039/C6QI00347H
_journal_volume                  3
_journal_year                    2016
_chemical_formula_moiety         'C6 Co K0.69 N6 Rb0.31, 2(C H6 N)'
_chemical_formula_sum            'C8 H12 Co K0.69 N8 Rb0.31'
_chemical_formula_weight         332.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-08-24 deposited with the CCDC.
2016-10-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.73(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.711(3)
_cell_length_b                   7.8880(16)
_cell_length_c                   13.717(3)
_cell_measurement_reflns_used    1606
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0.498
_cell_measurement_theta_min      0.455
_cell_volume                     1405.0(6)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku, SCXmini'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4754
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.476
_diffrn_reflns_theta_min         3.022
_exptl_absorpt_coefficient_mu    2.489
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             670.3
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.796
_refine_diff_density_min         -1.913
_refine_diff_density_rms         0.154
_refine_ls_extinction_coef       0.015(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     87
_refine_ls_number_reflns         1601
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0571
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0873P)²+9.4014P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1694
_refine_ls_wR_factor_ref         0.1727
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1467
_reflns_number_total             1606
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6qi00347h2.cif
_cod_data_source_block           2-298K
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4349541
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
C1 C 0.6859(3) 0.1249(5) 0.8776(3) 0.0273(9) Uani 1 1 d . . .
C2 C 0.8655(3) 0.2916(5) 0.9553(3) 0.0235(8) Uani 1 1 d . . .
C3 C 0.8106(3) 0.0448(5) 1.0651(3) 0.0239(8) Uani 1 1 d . . .
C4 C 0.0980(5) 0.1310(7) 0.1425(5) 0.0506(14) Uani 1 1 d . . .
H4D H 0.1460 0.1038 0.2087 0.076 Uiso 1 1 calc R U .
H4E H 0.0968 0.0408 0.0951 0.076 Uiso 1 1 calc R U .
H4F H 0.0305 0.1448 0.1482 0.076 Uiso 1 1 calc R U .
Co1 Co 0.7500 0.2500 1.0000 0.0172(3) Uani 1 2 d S . P
K1 K 0.5000 -0.21527(17) 0.7500 0.0408(4) Uani 0.69 2 d S T P
N1 N 0.6487(4) 0.0489(6) 0.8048(3) 0.0485(12) Uani 1 1 d . . .
N2 N 0.9349(3) 0.3182(5) 0.9287(3) 0.0336(9) Uani 1 1 d . . .
N3 N 0.8437(3) -0.0808(5) 1.1033(3) 0.0383(10) Uani 1 1 d . . .
N4 N 0.1295(3) 0.2886(6) 0.1048(3) 0.0340(9) Uani 1 1 d . . .
H4A H 0.1371 0.3696 0.1519 0.051 Uiso 1 1 calc R U .
H4B H 0.0815 0.3197 0.0467 0.051 Uiso 1 1 calc R U .
H4C H 0.1890 0.2725 0.0931 0.051 Uiso 1 1 calc R U .
Rb1 Rb 0.5000 -0.21527(17) 0.7500 0.0408(4) Uani 0.31 2 d S T P
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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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
N1 C1 Co1 179.2(5) . .
N2 C2 Co1 179.4(4) . .
N3 C3 Co1 177.6(4) . .
N4 C4 H4D 109.5 . .
N4 C4 H4E 109.5 . .
H4D C4 H4E 109.5 . .
N4 C4 H4F 109.5 . .
H4D C4 H4F 109.5 . .
H4E C4 H4F 109.5 . .
C2 Co1 C2 180.0 . 7_657
C2 Co1 C1 89.94(18) . 7_657
C2 Co1 C1 90.06(18) 7_657 7_657
C2 Co1 C1 90.06(18) . .
C2 Co1 C1 89.94(18) 7_657 .
C1 Co1 C1 180.0 7_657 .
C2 Co1 C3 90.85(17) . .
C2 Co1 C3 89.15(17) 7_657 .
C1 Co1 C3 91.07(17) 7_657 .
C1 Co1 C3 88.93(18) . .
C2 Co1 C3 89.15(17) . 7_657
C2 Co1 C3 90.85(17) 7_657 7_657
C1 Co1 C3 88.93(18) 7_657 7_657
C1 Co1 C3 91.07(17) . 7_657
C3 Co1 C3 180.0(2) . 7_657
N1 K1 N1 85.7(2) 2_656 .
N1 K1 N2 76.46(12) 2_656 3_445
N1 K1 N2 95.72(13) . 3_445
N1 K1 N2 95.72(13) 2_656 4_646
N1 K1 N2 76.46(12) . 4_646
N2 K1 N2 169.49(18) 3_445 4_646
N1 K1 N3 85.18(14) 2_656 8_445
N1 K1 N3 153.52(13) . 8_445
N2 K1 N3 106.18(12) 3_445 8_445
N2 K1 N3 79.79(12) 4_646 8_445
N1 K1 N3 153.52(13) 2_656 7_647
N1 K1 N3 85.18(14) . 7_647
N2 K1 N3 79.79(12) 3_445 7_647
N2 K1 N3 106.18(12) 4_646 7_647
N3 K1 N3 112.84(19) 8_445 7_647
C1 N1 K1 134.6(4) . .
C2 N2 Rb1 140.6(3) . 3
C2 N2 K1 140.6(3) . 3
Rb1 N2 K1 0.0 3 3
C3 N3 Rb1 153.0(4) . 7_647
C3 N3 K1 153.0(4) . 7_647
Rb1 N3 K1 0.0 7_647 7_647
C4 N4 H4A 109.5 . .
C4 N4 H4B 109.5 . .
H4A N4 H4B 109.5 . .
C4 N4 H4C 109.5 . .
H4A N4 H4C 109.5 . .
H4B N4 H4C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.136(6) .
C1 Co1 1.902(4) .
C2 N2 1.143(6) .
C2 Co1 1.901(4) .
C3 N3 1.144(6) .
C3 Co1 1.906(4) .
C4 N4 1.464(7) .
C4 H4D 0.9600 .
C4 H4E 0.9600 .
C4 H4F 0.9600 .
Co1 C2 1.901(4) 7_657
Co1 C1 1.902(4) 7_657
Co1 C3 1.906(4) 7_657
K1 N1 2.842(4) 2_656
K1 N1 2.842(5) .
K1 N2 2.877(4) 3_445
K1 N2 2.877(4) 4_646
K1 N3 2.909(4) 8_445
K1 N3 2.909(4) 7_647
N2 Rb1 2.877(4) 3
N2 K1 2.877(4) 3
N3 Rb1 2.909(4) 7_647
N3 K1 2.909(4) 7_647
N4 H4A 0.8900 .
N4 H4B 0.8900 .
N4 H4C 0.8900 .
