Slider-crank Mechanism in a Molecular Crystal: Conversion of Linear Thermal Expansion of Lattice to Circular Rotation of Coordination Chain
Tsunashima, Ryo; Fujikawa, Naomi; Shiga, Misaki; Miyagawa, Sayu; Ohno, Shiori; Masuya-Suzuki, Atsuko; Takahashi, Kiyonori; Nakamura, Takayoshi; Akutagawa, Tomoyuki; Nishihara, Sadafumi; CrystEngComm  (2022) –; doi:10.1039/D2CE00768A

data_7245157
_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_moiety         'C9 H12 Co1 K1 N5 O3'
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2020-10-05
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_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                   10.4530(5)
_cell_length_b                   10.4530(5)
_cell_length_c                   7.1875(3)
_cell_measurement_reflns_used    2024
_cell_measurement_temperature    303
_cell_measurement_theta_max      27.8660
_cell_measurement_theta_min      2.2160
_cell_volume                     680.13(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      303
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     48.00  93.00   0.50    0.16    --   21.85-178.00 150.00   90
  2  \w    -41.00  30.00   0.50    0.16    --   21.85  40.00 149.00  142
  3  \w     71.00 104.00   0.50    0.16    --   21.85  40.00 149.00   66
  4  \w     50.00 103.00   0.50    0.16    --   21.85 178.00-180.00  106
  5  \w     -5.00  59.00   0.50    0.16    --  -21.77  19.00-120.00  128
  6  \w    -87.00  -3.00   0.50    0.16    --  -21.77 110.00-129.00  168
  7  \w    -72.00 -46.00   0.50    0.16    --  -21.77 178.00-120.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0018589000
_diffrn_orient_matrix_UB_12      0.0154069000
_diffrn_orient_matrix_UB_13      -0.0963788000
_diffrn_orient_matrix_UB_21      0.0735906000
_diffrn_orient_matrix_UB_22      0.0137898000
_diffrn_orient_matrix_UB_23      -0.0050869000
_diffrn_orient_matrix_UB_31      -0.0267661000
_diffrn_orient_matrix_UB_32      -0.0755935000
_diffrn_orient_matrix_UB_33      -0.0205063000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       13
_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            4236
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.104
_diffrn_reflns_theta_min         2.250
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.578
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_description       block
_exptl_crystal_F_000             342
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.266
_exptl_crystal_size_min          0.221
_refine_diff_density_max         0.188
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
;
 Flack x determined using 193 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(3)
_refine_ls_extinction_coef       0.010(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     36
_refine_ls_number_reflns         605
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0279
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0235P)^2^+0.2383P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0648
_refine_ls_wR_factor_ref         0.0682
_reflns_Friedel_coverage         0.685
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.872
_reflns_number_gt                503
_reflns_number_total             605
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00768a2.cif
_cod_data_source_block           303k
_cod_original_cell_volume        680.13(7)
_cod_database_code               7245157
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C9H12N5O3CoK
_shelx_estimated_absorpt_t_max   0.722
_shelx_estimated_absorpt_t_min   0.658
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
;
_shelx_res_checksum              64121
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.851
_oxdiff_exptl_absorpt_empirical_full_min 0.455