Towards blue emitting monocyclometalated gold(iii) complexes - synthesis, characterization and photophysical investigations.
Bachmann, Michael; Fessler, Reto; Blacque, Olivier; Venkatesan, Koushik; Dalton transactions (Cambridge, England : 2003) 48 (2019) 7320–7330; doi:10.1039/c8dt05034a

data_7048984
_publ_section_title
;
 Towards blue emitting monocyclometalated gold(iii) complexes - synthesis,
 characterization and photophysical investigations.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7320
_journal_page_last               7330
_journal_paper_doi               10.1039/c8dt05034a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         '2(C24 H7 Au F13 N O), C H2 Cl2'
_chemical_formula_sum            'C49 H16 Au2 Cl2 F26 N2 O2'
_chemical_formula_weight         1623.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-09-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-24 deposited with the CCDC.
2019-02-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.7787(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.52497(10)
_cell_length_b                   20.3047(3)
_cell_length_c                   17.2623(3)
_cell_measurement_reflns_used    21299
_cell_measurement_temperature    183(1)
_cell_measurement_theta_max      32.4370
_cell_measurement_theta_min      2.3110
_cell_volume                     2636.27(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.13a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.13a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.13a (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015b)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      183(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3801
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.999
_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    -14.00  98.00   1.00   12.00    --   19.46  77.00-120.00  112
  2  \w    -14.00  98.00   1.00   12.00    --   19.46  77.00   0.00  112
  3  \w    -54.00  58.00   1.00   12.00    --  -20.40  77.00   0.00  112
  4  \w    -54.00  58.00   1.00   12.00    --  -20.40  77.00 120.00  112
  5  \w    -54.00  58.00   1.00   12.00    --  -20.40  77.00  90.00  112
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0407951000
_diffrn_orient_matrix_UB_12      0.0305447000
_diffrn_orient_matrix_UB_13      -0.0095900000
_diffrn_orient_matrix_UB_21      0.0199565000
_diffrn_orient_matrix_UB_22      -0.0048434000
_diffrn_orient_matrix_UB_23      -0.0395042000
_diffrn_orient_matrix_UB_31      -0.0826080000
_diffrn_orient_matrix_UB_32      -0.0162441000
_diffrn_orient_matrix_UB_33      -0.0062131000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            42242
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.505
_diffrn_reflns_theta_min         2.328
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.794
_exptl_absorpt_correction_T_max  0.719
_exptl_absorpt_correction_T_min  0.314
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.13a (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.045
_exptl_crystal_description       plate
_exptl_crystal_F_000             1532
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.758
_refine_diff_density_min         -1.145
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         8035
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0259
_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^)+(0.0322P)^2^+4.7969P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0710
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7035
_reflns_number_total             8035
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt05034a2.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 7048983--7048998.cif.'
_cod_original_cell_volume        2636.27(6)
_cod_database_code               7048984
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.687
_shelx_estimated_absorpt_t_min   0.294
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl1A-C25A = Cl2A-C25A = Cl1B-C25B = Cl2B-C25B
 1.78 with sigma of 0.01
 Cl1A-Cl2A = Cl1B-Cl2B
 2.9 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C25A) \\sim Ueq, Uanis(C25B) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(Cl1A) = Uanis(Cl2A) = Uanis(C25A)
Uanis(Cl1B) = Uanis(Cl2B) = Uanis(C25B)
4. Others
 Sof(C25B)=Sof(H25C)=Sof(H25D)=Sof(Cl1B)=Sof(Cl2B)=0.5*(1-FVAR(2))
 Sof(C25A)=Sof(H25B)=Sof(H25A)=Sof(Cl1A)=Sof(Cl2A)=0.5*FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C25A(H25B,H25A), C25B(H25C,H25D)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C8(H8), C10(H10), C11(H11)
;
_shelx_res_checksum              60792
_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.332
_oxdiff_exptl_absorpt_empirical_full_min 0.652