Augmenting metallobasicity to modulate gold hydrogen bonding
Maltz, Logan T.; Wilkins, Lewis C.; Gabbaï, François P.; Chemical Communications  (2022) –; doi:10.1039/D2CC03328C

data_7130502
_publ_section_title
;
 Augmenting metallobasicity to modulate gold hydrogen bonding
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC03328C
_journal_year                    2022
_chemical_formula_moiety         'C37 H30 Au O P, C0.5 H Cl'
_chemical_formula_sum            'C37.5 H31 Au Cl O P'
_chemical_formula_weight         761.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-07-21
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-07-21 deposited with the CCDC.	2022-07-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.4180(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.9800(3)
_cell_length_b                   10.22910(10)
_cell_length_c                   31.7739(3)
_cell_measurement_reflns_used    32418
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      31.4120
_cell_measurement_theta_min      2.0740
_cell_volume                     6046.76(13)
_computing_cell_refinement       'CrysAlisPro 1.171.42.61a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.61a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.61a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.952
_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    -97.14 153.86   1.00   10.00    --  -35.80  73.83  54.22  251
  2  \w    -97.14 153.86   1.00   10.00    --  -35.80  73.83-145.78  251
  3  \w    -97.14 153.86   1.00   10.00    --  -35.80  73.83 -65.78  251
  4  \w    -97.14 153.86   1.00   10.00    --  -35.80  73.83 -25.78  251
  5  \w    -86.89 164.11   1.00   10.00    --  -25.56  73.83  94.22  251
  6  \w    -86.89 164.11   1.00   10.00    --  -25.56  73.83-105.78  251
  7  \w    -97.14 153.86   1.00   10.00    --  -35.80  73.83 174.22  251
  8  \w    -97.14 153.86   1.00   10.00    --  -35.80  73.83  14.22  251
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0162268000
_diffrn_orient_matrix_UB_12      -0.0626041000
_diffrn_orient_matrix_UB_13      -0.0009114000
_diffrn_orient_matrix_UB_21      0.0342749000
_diffrn_orient_matrix_UB_22      -0.0290043000
_diffrn_orient_matrix_UB_23      0.0069121000
_diffrn_orient_matrix_UB_31      -0.0036977000
_diffrn_orient_matrix_UB_32      0.0066010000
_diffrn_orient_matrix_UB_33      0.0217026000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0551
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            125551
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.158
_diffrn_reflns_theta_min         2.096
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.037
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66999
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.61a (Rigaku Oxford Diffraction, 2022)
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    1.672
_exptl_crystal_description       block
_exptl_crystal_F_000             3000
_exptl_crystal_size_max          0.275
_exptl_crystal_size_mid          0.249
_exptl_crystal_size_min          0.083
_refine_diff_density_max         1.214
_refine_diff_density_min         -1.881
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         10969
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+15.3664P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0696
_refine_ls_wR_factor_ref         0.0831
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7709
_reflns_number_total             10969
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03328c2.cif
_cod_data_source_block           ltm_auph_revision_cold2_retryagain
_cod_original_formula_sum        'C37.50 H31 Au Cl O P'
_cod_database_code               7130502
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C37 H30 Au1 O1 P1'
_olex2_refinement_description
;
1. Restrained distances
 Cl1A-C38 \\sim C38-Cl1B
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Cl1A \\sim Cl1B: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 2A
3. Others
 Sof(Cl1B)=1-FVAR(1)
 Sof(Cl1A)=FVAR(1)
 Fixed Sof: H38A(0.5) H38B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C38(H38A,H38B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22),
  C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30),
 C33(H33), C34(H34), C35(H35), C36(H36), C37(H37)
;
_shelx_res_checksum              92026
_shelx_hkl_checksum              49309
_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 1.400
_oxdiff_exptl_absorpt_empirical_full_min 0.735