Anisotropic strain release in a thermosalient crystal: Correlation between the microscopic orientation of molecular rearrangements and the macroscopic mechanical motion
Seki, Tomohiro; Mashimo, Takaki; Ito, Hajime; Chemical Science  (2019) –; doi:10.1039/C8SC05563G

data_1550718
_publ_section_title
;
 Anisotropic strain release in a thermosalient crystal: Correlation
 between the microscopic orientation of molecular rearrangements and the
 macroscopic mechanical motion
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC05563G
_journal_year                    2019
_chemical_formula_moiety         'C27 H19 Au Cl N'
_chemical_formula_sum            'C27 H19 Au Cl N'
_chemical_formula_weight         589.85
_chemical_name_systematic        1_-50C
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-08-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-11 deposited with the CCDC.    2019-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.005(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6176(3)
_cell_length_b                   11.5301(3)
_cell_length_c                   17.0283(5)
_cell_measurement_reflns_used    10705
_cell_measurement_temperature    223
_cell_measurement_theta_max      28.5890
_cell_measurement_theta_min      3.0740
_cell_volume                     2169.28(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      223
_diffrn_detector                 'PLATUS 200K area detector'
_diffrn_detector_area_resol_mean 5.811
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.866
_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    -19.00   6.00   0.50    0.60    --    5.00  45.00 -13.00   50
  2  \w    -32.00  -7.00   0.50    0.60    --   -7.40  45.00 -13.00   50
  3  \w    -97.00 -49.00   0.50    0.60    --   -7.40  29.00 -90.00   96
  4  \w    -26.00   0.00   0.50    0.60    --   -7.40  29.00 -90.00   52
  5  \w     35.00  82.00   0.50    0.60    --   -7.40  29.00 -90.00   94
  6  \w    -88.00  66.00   0.50    0.60    --   -7.40  29.00  60.00  308
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0632478000
_diffrn_orient_matrix_UB_12      0.0099521000
_diffrn_orient_matrix_UB_13      -0.0107837000
_diffrn_orient_matrix_UB_21      0.0101067000
_diffrn_orient_matrix_UB_22      0.0424346000
_diffrn_orient_matrix_UB_23      0.0316055000
_diffrn_orient_matrix_UB_31      0.0046049000
_diffrn_orient_matrix_UB_32      0.0433929000
_diffrn_orient_matrix_UB_33      -0.0283483000
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.866
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19544
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.866
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.993
_diffrn_reflns_theta_min         3.074
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              micromax007
_exptl_absorpt_coefficient_mu    6.918
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40338
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_description       block
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.982
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.878
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4990
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.878
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0263
_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/[\s^2^(Fo^2^)+(0.0553P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0680
_refine_ls_wR_factor_ref         0.0720
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4261
_reflns_number_total             4990
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc05563g2.cif
_cod_data_source_block           msm-178_-50deg
_cod_database_code               1550718
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C H N Au Cl'
_shelx_estimated_absorpt_t_max   0.724
_shelx_estimated_absorpt_t_min   0.231
_reflns_odcompleteness_completeness 98.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C005(H005), C009(H009), C00B(H00B), C00C(H00C), C00E(H00E), C00F(H00F),
 C00H(H00H), C00I(H00I), C00J(H00J), C00K(H00K), C00M(H00M), C00N(H00N),
 C00O(H00O), C00P(H00P), C00Q(H00Q), C00R(H00R), C00S(H00S), C00T(H00T),
 C00U(H00U)
;
_shelx_res_checksum              30569
_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 1.817
_oxdiff_exptl_absorpt_empirical_full_min 0.702