Synthesis and characterization of N-heterocyclic carbene-MOEt<sub>2</sub> complexes (M = Cu, Ag, Au). Analysis of solvated auxiliary-ligand free [(NHC)M]<sup>+</sup> species.
Muñoz-Castro, Alvaro; Wang, Guocang; Ponduru, Tharun Teja; Dias, H. V. Rasika; Physical chemistry chemical physics : PCCP 23 (2021) 1577–1583; doi:10.1039/d0cp05222a

data_7241702
_publ_section_title
;
 Synthesis and characterization of N-heterocyclic carbene-MOEt<sub>2</sub>
 complexes (M = Cu, Ag, Au). Analysis of solvated auxiliary-ligand free
 [(NHC)M]<sup>+</sup> species.
;
_journal_issue                   2
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              1577
_journal_page_last               1583
_journal_paper_doi               10.1039/d0cp05222a
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C22 H37 Au N O, F6 Sb'
_chemical_formula_sum            'C22 H37 Au F6 N O Sb'
_chemical_formula_weight         764.24
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-15 deposited with the CCDC.	2020-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.9320(5)
_cell_length_b                   16.4501(6)
_cell_length_c                   24.4593(9)
_cell_measurement_reflns_used    9753
_cell_measurement_temperature    100.01
_cell_measurement_theta_max      33.29
_cell_measurement_theta_min      2.61
_cell_volume                     5203.3(3)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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      100.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            81547
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.325
_diffrn_reflns_theta_min         2.605
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.728
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.4888
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1274 before and 0.0602 after correction. The Ratio of minimum to maximum transmission is 0.6548. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.951
_exptl_crystal_description       parallelpipeds
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.168
_refine_diff_density_min         -0.803
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       0.000148(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         10017
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0233
_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^)+(0.0120P)^2^+8.1320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0427
_refine_ls_wR_factor_ref         0.0458
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8342
_reflns_number_total             10017
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cp05222a2.cif
_cod_data_source_block           rad748_0m_a
_cod_depositor_comments
'Adding full bibliography for 7241701--7241703.cif.'
_cod_database_code               7241702
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.650
_shelx_estimated_absorpt_t_min   0.412
_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.a Rotating group:
 O(HA,HB)
2.b Ternary CH refined with riding coordinates:
 C11(H11), C14(H14)
2.c Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C19(H19A,H19B), C21(H21A,H21B)
2.d Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9)
2.e Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C22(H22A,
 H22B,H22C)
;
_shelx_res_checksum              4463
_olex2_submission_special_instructions 'No special instructions were received'