Mixed crystal formation of two gold isocyanide complexes with various ratios for continuous tuning of photophysical properties.
Seki, Tomohiro; Toyoshima, Naoki; Ito, Hajime; Dalton transactions (Cambridge, England : 2003) 49 (2020) 2073–2076; doi:10.1039/d0dt00195c

data_7703361
_publ_section_title
;
 Mixed crystal formation of two gold isocyanide complexes with various
 ratios for continuous tuning of photophysical properties.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2073
_journal_page_last               2076
_journal_paper_doi               10.1039/d0dt00195c
_journal_volume                  49
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C20 H23 Au F4 N2 Si'
_chemical_formula_sum            'C20 H23 Au F4 N2 Si'
_chemical_formula_weight         592.46
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-08-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-14 deposited with the CCDC.	2020-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.20410(10)
_cell_length_b                   13.5498(2)
_cell_length_c                   21.8640(3)
_cell_measurement_reflns_used    8428
_cell_measurement_temperature    150
_cell_measurement_theta_max      75.5370
_cell_measurement_theta_min      3.8310
_cell_volume                     2134.23(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45h (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45h (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45h (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      150
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.982
_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     24.00 118.00   0.50    0.05    --   42.80  47.00  90.00  188
  2  \w   -156.00-119.00   0.50    0.06    --  -84.50 -95.00  83.00   74
  3  \w   -142.00 -85.00   0.50    0.06    --  -84.50 -85.00-179.00  114
  4  \w    132.00 173.00   0.50    0.06    --  108.63  47.00  90.00   82
  5  \w     93.00 126.00   0.50    0.06    --  108.63  47.00  90.00   66
  6  \w   -115.00 -70.00   0.50    0.05    --  -42.80-125.00  90.00   90
  7  \w   -113.00 -73.00   0.50    0.05    --  -42.80-125.00  60.00   80
  8  \w     72.00 115.00   0.50    0.05    --   42.80 125.00  30.00   86
  9  \w     43.00  77.00   0.50    0.06    --  108.63 -45.00-150.00   68
 10  \w     35.00  69.00   0.50    0.06    --  108.63 -94.00 -60.00   68
 11  \w     75.00 101.00   0.50    0.06    --  108.63 -94.00 -60.00   52
 12  \w     90.00 166.00   0.50    0.06    --  108.63  77.00-120.00  152
 13  \w     37.00  66.00   0.50    0.06    --  108.63 -30.00-180.00   58
 14  \w     72.00 110.00   0.50    0.06    --  108.63-125.00  90.00   76
 15  \w    108.00 134.00   0.50    0.06    --  108.63 -85.00-179.00   52
 16  \w     30.00  55.00   0.50    0.06    --  108.63 -30.00-150.00   50
 17  \w     40.00  65.00   0.50    0.06    --  108.63 -45.00 150.00   50
 18  \w     35.00  60.00   0.50    0.06    --  108.63 -45.00 -90.00   50
 19  \w     30.00  66.00   0.50    0.06    --  108.63 -30.00   0.00   72
 20  \w     37.00  66.00   0.50    0.06    --  108.63 -45.00-180.00   58
 21  \w     30.00  55.00   0.50    0.06    --  108.63 -30.00 120.00   50
 22  \w     39.00  92.00   0.50    0.06    --  108.63 -85.00-179.00  106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1208490000
_diffrn_orient_matrix_UB_12      -0.0792468000
_diffrn_orient_matrix_UB_13      -0.0311620000
_diffrn_orient_matrix_UB_21      -0.0355195000
_diffrn_orient_matrix_UB_22      0.0707184000
_diffrn_orient_matrix_UB_23      -0.0539673000
_diffrn_orient_matrix_UB_31      0.1726433000
_diffrn_orient_matrix_UB_32      -0.0409570000
_diffrn_orient_matrix_UB_33      -0.0327938000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            11641
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.883
_diffrn_reflns_theta_min         3.838
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.873
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66255
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45h (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.844
_exptl_crystal_description       needle
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_min          0.069
_refine_diff_density_max         0.945
_refine_diff_density_min         -1.111
_refine_diff_density_rms         0.186
_refine_ls_abs_structure_details
;
 Flack x determined using 1731 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.037(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         4287
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0453P)^2^+1.7257P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0855
_reflns_Friedel_coverage         0.714
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.945
_reflns_number_gt                4225
_reflns_number_total             4287
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00195c2.cif
_cod_data_source_block           tys-336-1
_cod_depositor_comments
'Adding full bibliography for 7703359--7703361.cif.'
_cod_database_code               7703361
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'Au Si N F H C'
_shelx_estimated_absorpt_t_max   0.448
_shelx_estimated_absorpt_t_min   0.230
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7)
2.b Fitted hexagon refined as free rotating group:
 C23(C22,C21,N20,C19,C24), C3(C4,C5,C6,C7,C2)
2.c Idealised Me refined as rotating group:
 C13(H13a,H13b,H13c), C12(H12a,H12b,H12c), C14(H14a,H14b,H14c), C18(H18a,H18b,
 H18c), C10(H10a,H10b,H10c), C11(H11a,H11b,H11c), C17(H17a,H17b,H17c)
;
_shelx_res_checksum              11613
_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 1.397
_oxdiff_exptl_absorpt_empirical_full_min 0.745