Synthesis of hydroxyl-functionalized N-heterocyclic carbene gold(i) complexes and peptide conjugates.
Diehl, Tobias; Krause, Melanie T. S.; Ueberlein, Sven; Becker, Stefanie; Trommer, Aline; Schnakenburg, Gregor; Engeser, Marianne; Dalton transactions (Cambridge, England : 2003) 46 (2017) 2988–2997; doi:10.1039/c6dt04834j

data_7042005
_publ_section_title
;
 Synthesis of hydroxyl-functionalized N-heterocyclic carbene gold(i)
 complexes and peptide conjugates.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2988
_journal_page_last               2997
_journal_paper_doi               10.1039/c6dt04834j
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C12 H20 Au N4 O2, F6 P'
_chemical_formula_sum            'C12 H20 Au F6 N4 O2 P'
_chemical_formula_weight         594.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-01-10
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_audit_update_record
;
2017-01-18 deposited with the CCDC.
2017-02-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 124.758(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.423(4)
_cell_length_b                   12.458(2)
_cell_length_c                   10.897(2)
_cell_measurement_reflns_used    9905
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.86
_cell_measurement_theta_min      2.542
_cell_volume                     1831.7(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 9
_diffrn_detector_type            'area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0915
_diffrn_reflns_av_unetI/netI     0.1067
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2078
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.993
_diffrn_reflns_theta_min         3.019
_diffrn_source                   'sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.192
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.3926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1369 before and 0.1024 after correction.
 The Ratio of minimum to maximum transmission is 0.53.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 41088 reflections, Rint = 0.1196
 (22234 with I > 3sig(I), Rint = 0.0955)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.155
_exptl_crystal_description       plate
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.256
_refine_diff_density_min         -2.036
_refine_diff_density_rms         0.262
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         2078
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0407
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0356P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.0984
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1620
_reflns_number_total             2078
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04834j2.cif
_cod_data_source_block           2586
_cod_depositor_comments
'Adding full bibliography for 7042003--7042010.cif.'
_cod_database_code               7042005
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.735
_shelx_estimated_absorpt_t_min   0.291
_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, All O(H,H) groups
2. Others
 Fixed Sof: H1B(0.5) H1A(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5)
3.c Tetrahedral OH refined as rotating group:
 O1(H1B), O1(H1A)
3.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
;
_shelx_res_checksum              60178
_olex2_submission_special_instructions 'No special instructions were received'