#------------------------------------------------------------------------------
#$Date: 2022-07-23 01:29:16 +0200 (Sat 23 de Jul de 2022) $
#$Revision: 276812 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/51/7245156.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_7245156
loop_
_publ_author_name
'Tsunashima, Ryo'
'Fujikawa, Naomi'
'Shiga, Misaki'
'Miyagawa, Sayu'
'Ohno, Shiori'
'Masuya-Suzuki, Atsuko'
'Takahashi, Kiyonori'
'Nakamura, Takayoshi'
'Akutagawa, Tomoyuki'
'Nishihara, Sadafumi'
_publ_section_title
;
 Slider-crank Mechanism in a Molecular Crystal: Conversion of Linear
 Thermal Expansion of Lattice to Circular Rotation of Coordination Chain
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00768A
_journal_year                    2022
_chemical_formula_sum            'C9 H12 Co K N5 O3'
_chemical_formula_weight         336.27
_space_group_crystal_system      hexagonal
_space_group_IT_number           190
_space_group_name_Hall           'P -6c -2c'
_space_group_name_H-M_alt        'P -6 2 c'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-03-17 deposited with the CCDC.	2022-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   10.5556(6)
_cell_length_b                   10.5556(6)
_cell_length_c                   7.2239(3)
_cell_measurement_reflns_used    2093
_cell_measurement_temperature    390
_cell_measurement_theta_max      27.5730
_cell_measurement_theta_min      2.2010
_cell_volume                     697.06(6)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      390
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1077
_diffrn_reflns_av_unetI/netI     0.0530
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4706
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        28.500
_diffrn_reflns_theta_max         28.907
_diffrn_reflns_theta_min         2.228
_exptl_absorpt_coefficient_mu    1.540
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_description       block
_exptl_crystal_F_000             342
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
;
 Flack x determined using 179 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     35
_refine_ls_number_reflns         618
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0452
_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)+(0.0805P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1161
_refine_ls_wR_factor_ref         0.1259
_reflns_Friedel_coverage         0.698
_reflns_Friedel_fraction_full    0.937
_reflns_Friedel_fraction_max     0.891
_reflns_number_gt                495
_reflns_number_total             618
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2ce00768a2.cif
_cod_data_source_block           390k
_cod_original_cell_volume        697.06(8)
_cod_database_code               7245156
_shelx_shelxl_version_number     2018/3
_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.
;
_shelx_res_file
;
TITL 423k_a.res in P-62c
    423k.res
    created by SHELXL-2018/3 at 17:29:57 on 07-Oct-2020
REM Old TITL 423k in P6(3)mc
REM SHELXT solution in P-62c: R1 0.107, Rweak 0.005, Alpha 0.029
REM <I/s> 0.318 for 26 systematic absences, Orientation as input
REM Flack x = 0.109 ( 0.044 ) from 172 Parsons' quotients
REM Formula found by SHELXT: C12 N5 K Co
CELL 0.71073 10.5556 10.5556 7.2239 90 90 120
ZERR 2 0.0006 0.0006 0.0003 0 0 0
LATT -1
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM +X,+Y,0.5-Z
SYMM -Y,+X-Y,0.5-Z
SYMM +Y-X,-X,0.5-Z
SYMM +Y,+X,-Z
SYMM -Y+X,-Y,-Z
SYMM -X,-X+Y,-Z
SYMM +Y,+X,0.5+Z
SYMM -Y+X,-Y,0.5+Z
SYMM -X,-X+Y,0.5+Z
SFAC C H Co K N O
UNIT 18 24 2 2 10 6

L.S. 4
PLAN  5
CONF
MORE -1
BOND $H
fmap 2
acta 57
REM <olex2.extras>
REM <HklSrc "%.\\423k.hkl">
REM </olex2.extras>

WGHT    0.080500
FVAR       0.85633
CO1   3    0.666667    0.333333    0.750000    10.16667    0.04384    0.04384 =
         0.03796    0.00000    0.00000    0.02192
K2    4    1.000000    0.000000    1.000000    10.16667    0.06848    0.06848 =
         0.04772    0.00000    0.00000    0.03424
N3    5    0.666667    0.333333    0.430947    10.33333    0.04168    0.04168 =
         0.02746    0.00000    0.00000    0.02084
N5    5    0.739505    0.194445    0.750000    10.50000    0.10521    0.09457 =
         0.04076    0.00000    0.00000    0.07365
C4    1    0.617052    0.430733    0.355808    11.00000    0.09031    0.07387 =
         0.03380   -0.00364   -0.00322    0.05938
AFIX  23
H4A   2    0.680886    0.529484    0.400170    11.00000   -1.20000
H4B   2    0.518967    0.399221    0.400168    11.00000   -1.20000
AFIX   0
O1    6    0.837684    0.041818    0.750000    10.50000    0.18998    0.21791 =
         0.09629    0.00000    0.00000    0.17503
C6    1    0.790262    0.123465    0.750000    10.50000    0.08540    0.09816 =
         0.03832    0.00000    0.00000    0.07107
HKLF 4




REM  423k_a.res in P-62c
REM wR2 = 0.1259, GooF = S = 1.005, Restrained GooF = 1.005 for all data
REM R1 = 0.0452 for 495 Fo > 4sig(Fo) and 0.0574 for all 618 data
REM 35 parameters refined using 0 restraints

END

WGHT      0.0805      0.0000

REM Highest difference peak  0.402,  deepest hole -0.405,  1-sigma level  0.074
Q1    1   0.9876  0.1902  0.7500  10.50000  0.05    0.40
Q2    1   0.8267  0.2782  0.7500  10.50000  0.05    0.31
Q3    1   0.9415  0.2351  0.7500  10.50000  0.05    0.23
Q4    1   0.9014  0.2545  0.7500  10.50000  0.05    0.19
Q5    1   0.6420  0.6371  0.2500  10.50000  0.05    0.17
;
_shelx_res_checksum              76253
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x, y, -z+1/2'
'-y, x-y, -z+1/2'
'-x+y, -x, -z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, z+1/2'
'x-y, -y, z+1/2'
'-x, -x+y, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.666667 0.333333 0.750000 0.0419(4) Uani 1 6 d S T P . .
K2 K 1.000000 0.000000 1.000000 0.0616(6) Uani 1 6 d S T P . .
N3 N 0.666667 0.333333 0.4309(6) 0.0369(10) Uani 1 3 d S T P . .
N5 N 0.7395(8) 0.1944(8) 0.750000 0.070(2) Uani 1 2 d S T P . .
C4 C 0.6171(7) 0.4307(5) 0.3558(6) 0.0578(12) Uani 1 1 d . . . . .
H4A H 0.680886 0.529484 0.400170 0.069 Uiso 1 1 calc R U . . .
H4B H 0.518967 0.399221 0.400168 0.069 Uiso 1 1 calc R U . . .
O1 O 0.8377(10) 0.0418(11) 0.750000 0.136(4) Uani 1 2 d S T P . .
C6 C 0.7903(10) 0.1235(10) 0.750000 0.063(2) Uani 1 2 d S T P . .
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
Co1 0.0438(5) 0.0438(5) 0.0380(6) 0.000 0.000 0.0219(3)
K2 0.0685(9) 0.0685(9) 0.0477(11) 0.000 0.000 0.0342(5)
N3 0.0417(16) 0.0417(16) 0.0275(18) 0.000 0.000 0.0208(8)
N5 0.105(6) 0.095(5) 0.041(2) 0.000 0.000 0.074(6)
C4 0.090(3) 0.074(4) 0.0338(18) -0.004(2) -0.003(2) 0.059(3)
O1 0.190(9) 0.218(10) 0.096(5) 0.000 0.000 0.175(9)
C6 0.085(6) 0.098(6) 0.038(3) 0.000 0.000 0.071(6)
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'
Co Co 0.3494 0.9721 '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'
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
N5 Co1 N5 120.000(1) . 2_655 ?
N5 Co1 N5 120.000(1) . 3_665 ?
N5 Co1 N5 120.0 2_655 3_665 ?
N5 Co1 N3 90.0 . 4_556 ?
N5 Co1 N3 90.000(1) 2_655 4_556 ?
N5 Co1 N3 90.001(1) 3_665 4_556 ?
N5 Co1 N3 90.0 . . ?
N5 Co1 N3 90.000(1) 2_655 . ?
N5 Co1 N3 90.000(1) 3_665 . ?
N3 Co1 N3 180.0 4_556 . ?
O1 K2 O1 121.9(4) . 9_767 ?
O1 K2 O1 79.37(15) . 2_645 ?
O1 K2 O1 152.5(5) 9_767 2_645 ?
O1 K2 O1 152.5(5) . 7_647 ?
O1 K2 O1 79.37(15) 9_767 7_647 ?
O1 K2 O1 87.3(2) 2_645 7_647 ?
O1 K2 O1 87.3(2) . 8_557 ?
O1 K2 O1 79.37(15) 9_767 8_557 ?
O1 K2 O1 121.9(4) 2_645 8_557 ?
O1 K2 O1 79.37(15) 7_647 8_557 ?
O1 K2 O1 79.37(15) . 3_765 ?
O1 K2 O1 87.3(2) 9_767 3_765 ?
O1 K2 O1 79.37(15) 2_645 3_765 ?
O1 K2 O1 121.9(4) 7_647 3_765 ?
O1 K2 O1 152.5(5) 8_557 3_765 ?
O1 K2 K2 47.51(10) . 4_556 ?
O1 K2 K2 132.49(10) 9_767 4_556 ?
O1 K2 K2 47.51(10) 2_645 4_556 ?
O1 K2 K2 132.49(10) 7_647 4_556 ?
O1 K2 K2 132.49(10) 8_557 4_556 ?
O1 K2 K2 47.51(10) 3_765 4_556 ?
O1 K2 K2 132.49(10) . 4_557 ?
O1 K2 K2 47.51(10) 9_767 4_557 ?
O1 K2 K2 132.49(10) 2_645 4_557 ?
O1 K2 K2 47.51(10) 7_647 4_557 ?
O1 K2 K2 47.51(10) 8_557 4_557 ?
O1 K2 K2 132.49(10) 3_765 4_557 ?
K2 K2 K2 180.0 4_556 4_557 ?
C4 N3 C4 107.2(2) 3_665 2_655 ?
C4 N3 C4 107.2(2) 3_665 . ?
C4 N3 C4 107.2(2) 2_655 . ?
C4 N3 Co1 111.7(2) 3_665 . ?
C4 N3 Co1 111.7(2) 2_655 . ?
C4 N3 Co1 111.7(2) . . ?
C6 N5 Co1 175.3(8) . . ?
N3 C4 C4 111.7(2) . 4 ?
N3 C4 H4A 109.3 . . ?
C4 C4 H4A 109.3 4 . ?
N3 C4 H4B 109.3 . . ?
C4 C4 H4B 109.3 4 . ?
H4A C4 H4B 108.0 . . ?
C6 O1 K2 130.8(4) . . ?
C6 O1 K2 130.8(4) . 4_556 ?
K2 O1 K2 85.0(2) . 4_556 ?
N5 C6 O1 176.8(12) . . ?
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
Co1 N5 1.967(6) . ?
Co1 N5 1.967(6) 2_655 ?
Co1 N5 1.967(6) 3_665 ?
Co1 N3 2.305(4) 4_556 ?
Co1 N3 2.305(4) . ?
K2 O1 2.674(5) . ?
K2 O1 2.674(5) 9_767 ?
K2 O1 2.674(5) 2_645 ?
K2 O1 2.674(5) 7_647 ?
K2 O1 2.674(5) 8_557 ?
K2 O1 2.674(5) 3_765 ?
K2 K2 3.61195(15) 4_556 ?
K2 K2 3.61195(16) 4_557 ?
N3 C4 1.471(4) 3_665 ?
N3 C4 1.471(4) 2_655 ?
N3 C4 1.471(4) . ?
N5 C6 1.118(8) . ?
C4 C4 1.529(8) 4 ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
O1 C6 1.194(9) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C4 N3 C4 C4 57.4(2) 3_665 . . 4 ?
C4 N3 C4 C4 -57.4(2) 2_655 . . 4 ?
Co1 N3 C4 C4 180.000(1) . . . 4 ?
