Synthesis and characterisation of fluorescent aminophosphines and their coordination to gold(i).
Groves, Lara M.; Ward, Benjamin D.; Newman, Paul D.; Horton, Peter N.; Coles, Simon J.; Pope, Simon J. A.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 9324–9333; doi:10.1039/c8dt02256a

data_7046866
_publ_section_title
;
 Synthesis and characterisation of fluorescent aminophosphines and their
 coordination to gold(i).
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9324
_journal_page_last               9333
_journal_paper_doi               10.1039/c8dt02256a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C26 H18 Au Cl N O2 P'
_chemical_formula_sum            'C26 H18 Au Cl N O2 P'
_chemical_formula_weight         639.80
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-05-19
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-08-31 deposited with the CCDC.
2018-06-20 downloaded from the CCDC.
;
_cell_angle_alpha                90.9323(9)
_cell_angle_beta                 101.3732(9)
_cell_angle_gamma                94.2899(9)
_cell_formula_units_Z            4
_cell_length_a                   9.23605(10)
_cell_length_b                   14.82932(17)
_cell_length_c                   16.64944(19)
_cell_measurement_reflns_used    37661
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.1320
_cell_measurement_theta_min      2.2820
_cell_volume                     2228.21(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.999
_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    -39.00  77.00   1.00    2.00    --  -11.90  38.00 -90.00  116
  2  \w   -101.00  22.00   1.00    2.00    --  -11.90 -72.00   0.00  123
  3  \w   -101.00  22.00   1.00    2.00    --  -11.90 -72.00  90.00  123
  4  \w   -101.00  15.00   1.00    2.00    --  -11.90 -38.00-150.00  116
  5  \w    -39.00  77.00   1.00    2.00    --  -11.90  38.00-180.00  116
  6  \w    -46.00  77.00   1.00    2.00    --  -11.90  72.00 -30.00  123
  7  \w    -46.00  57.00   1.00    2.00    --  -11.90  72.00  90.00  103
  8  \w    -43.00  77.00   1.00    2.00    --  -11.90  57.00  30.00  120
;
_diffrn_measurement_device       'four-circle \k goniometer'
_diffrn_measurement_device_type
'Rigaku FRE+ equipped with HF Varimax confocal mirrors and an AFC12 goniometer and HG Saturn 724+ detector'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0480593000
_diffrn_orient_matrix_UB_12      -0.0197363000
_diffrn_orient_matrix_UB_13      0.0323530000
_diffrn_orient_matrix_UB_21      0.0026292000
_diffrn_orient_matrix_UB_22      -0.0379768000
_diffrn_orient_matrix_UB_23      -0.0259796000
_diffrn_orient_matrix_UB_31      0.0621200000
_diffrn_orient_matrix_UB_32      0.0217079000
_diffrn_orient_matrix_UB_33      -0.0129853000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, HF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            60900
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         2.497
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    6.819
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.692
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.9g (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.907
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.167
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.740
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         10204
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0197
_refine_ls_R_factor_gt           0.0176
_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^)+(0.0161P)^2^+1.8763P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0391
_refine_ls_wR_factor_ref         0.0399
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9595
_reflns_number_total             10204
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02256a2.cif
_cod_data_source_block           '[AuCl(L3)]'
_cod_depositor_comments          'Adding full bibliography for 7046866.cif.'
_cod_database_code               7046866
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C26 H18 N O2 P Cl Au'
_chemical_oxdiff_usercomment     LG313.2
_diffrn_oxdiff_ac3_digest_frames
;
01b494dd05ab17265b416f393a9d7f5bce0094079c1
;
_diffrn_oxdiff_ac3_digest_hkl
;
019df5c853547ea9161a7539f2fd403516cf0f
;
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C5(H5), C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14),
 C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24),
  C25(H25), C26(H26), N31(H31), C35(H35), C36(H36), C37(H37), C38(H38),
 C42(H42), C43(H43), C44(H44), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50),
  C52(H52), C53(H53), C54(H54), C55(H55), C56(H56)
;
_shelx_res_checksum              14975
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id LG313.2
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.471
_oxdiff_exptl_absorpt_empirical_full_min 0.744