Luminescent mechanochromism of gold N-heterocyclic carbene complexes with hypso- and bathochromic spectral shifts.
Seki, Tomohiro; Kashiyama, Kentaro; Ito, Hajime; Dalton transactions (Cambridge, England : 2003) 48 (2019) 7105–7109; doi:10.1039/c9dt00566h

data_7049453
_publ_section_title
;
 Luminescent mechanochromism of gold N-heterocyclic carbene complexes with
 hypso- and bathochromic spectral shifts.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7105
_journal_page_last               7109
_journal_paper_doi               10.1039/c9dt00566h
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C25 H25 Au N2, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C25.5 H25 Au Cl N2'
_chemical_formula_weight         591.89
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-11-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-04 deposited with the CCDC.    2019-03-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.537(2)
_cell_length_b                   10.2462(6)
_cell_length_c                   11.5862(10)
_cell_measurement_reflns_used    4866
_cell_measurement_temperature    93
_cell_measurement_theta_max      28.6710
_cell_measurement_theta_min      2.6670
_cell_volume                     2438.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.11a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.11a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.11a (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      93
_diffrn_detector                 'PLATUS 200K area detector'
_diffrn_detector_area_resol_mean 5.811
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.877
_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    -32.00  -7.00   0.50    2.53    --   -7.30  17.00 107.00   50
  2  \w      7.00  80.00   0.50    2.53    --   -7.30  57.00 150.00  146
  3  \w    -96.00 -18.00   0.50    2.53    --   -7.30  57.00 150.00  156
;
_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      0.0045181000
_diffrn_orient_matrix_UB_12      -0.0189233000
_diffrn_orient_matrix_UB_13      -0.0584373000
_diffrn_orient_matrix_UB_21      -0.0341692000
_diffrn_orient_matrix_UB_22      -0.0058084000
_diffrn_orient_matrix_UB_23      -0.0068003000
_diffrn_orient_matrix_UB_31      -0.0017904000
_diffrn_orient_matrix_UB_32      0.0662388000
_diffrn_orient_matrix_UB_33      -0.0173630000
_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  0.0824
_diffrn_reflns_av_unetI/netI     0.0548
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.877
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            12004
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.214
_diffrn_reflns_theta_min         1.983
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              micromax007
_exptl_absorpt_coefficient_mu    6.157
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.13621
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.11a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_description       plate
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.369
_exptl_crystal_size_mid          0.194
_exptl_crystal_size_min          0.072
_refine_diff_density_max         2.393
_refine_diff_density_min         -3.009
_refine_diff_density_rms         0.253
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         3049
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.1040
_refine_ls_R_factor_gt           0.0848
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0914P)^2^+48.8596P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2233
_refine_ls_wR_factor_ref         0.2402
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2340
_reflns_number_total             3049
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00566h2.cif
_cod_data_source_block           ksy-325-1_twin1_hklf4
_cod_depositor_comments          'Adding full bibliography for 7049453.cif.'
_cod_original_formula_sum        'C25.50 H25 Au Cl N2'
_cod_database_code               7049453
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C H Au N'
_shelx_estimated_absorpt_t_max   0.666
_shelx_estimated_absorpt_t_min   0.210
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C19-C12
 2.42 with sigma of 0.04
 C18-C17
 2.42 with sigma of 0.04
 C12-C16
 2.42 with sigma of 0.04
 C16-C19
 2.42 with sigma of 0.04
 C15-C18
 2.42 with sigma of 0.04
 C17-C15
 2.42 with sigma of 0.04
3. Restrained planarity
 C15, C17, C18, C16, C19, C12
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C20 \\sim Cl1 \\sim Cl2: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C15 \\sim C16 \\sim C17 \\sim C12 \\sim C18 \\sim C19: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 C20, Cl1, Cl2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C18, C12, C17, C16, C15, C19
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C17(0.25) H17(0.25) C16(0.25) H16(0.25) H15(0.25) H15A(0.25)
 C19(0.25) H19(0.25) C18(0.25) H18(0.25) C13(0.5) H13(0.5) C14(0.5) H14(0.5)
 Cl1(0.25) Cl2(0.25) C20(0.25) H20A(0.25) H20B(0.25)
7.a Free rotating group:
 Cl1(Cl2,C20)
7.b Ternary CH refined with riding coordinates:
 C7(H7)
7.c Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B)
7.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C17(H17), C16(H16), C15(H15), C15(H15A), C19(H19),
 C18(H18), C13(H13), C14(H14)
7.e Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              40597
_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 3.129
_oxdiff_exptl_absorpt_empirical_full_min 0.387
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
_twin_special_details
;
Component 2 rotated by -179.8861\% 
 around [1.00 -0.04 -0.01] (reciprocal) or [0.99 -0.17 -0.04] (direct)
;