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_7241701
_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         'F6 Sb, C27 H40 Cu N2 O, 0.5(H2 O)'
_chemical_formula_sum            'C27 H41 Cu F6 N2 O1.5 Sb'
_chemical_formula_weight         716.91
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-15
_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                120
_cell_formula_units_Z            18
_cell_length_a                   27.8000(10)
_cell_length_b                   27.8000(10)
_cell_length_c                   21.5997(8)
_cell_measurement_reflns_used    9635
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.41
_cell_measurement_theta_min      2.93
_cell_volume                     14456.7(9)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 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      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Bruker D8 Quest with a Photon 100 CMOS detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            56564
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.279
_diffrn_reflns_theta_min         2.927
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.560
_exptl_absorpt_correction_T_max  0.3368
_exptl_absorpt_correction_T_min  0.2654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0831 before and 0.0639 after correction. The Ratio of minimum to maximum transmission is 0.7880. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_description       rods
_exptl_crystal_F_000             6534
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.847
_refine_diff_density_min         -0.787
_refine_diff_density_rms         0.107
_refine_ls_abs_structure_details
;
 Flack x determined using 3524 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.010(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         7972
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0567P)^2^+67.0215P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0960
_refine_ls_wR_factor_ref         0.0982
_reflns_Friedel_coverage         0.995
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                7533
_reflns_number_total             7972
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cp05222a2.cif
_cod_data_source_block           rad744_0m_a
_cod_depositor_comments
'Adding full bibliography for 7241701--7241703.cif.'
_cod_original_cell_volume        14456.7(12)
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_original_formula_sum        'C27 H41 Cu F6 N2 O1.50 Sb'
_cod_database_code               7241701
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.872
_shelx_estimated_absorpt_t_min   0.567
_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: O2(0.5) H2C(0.5) H2D(0.5)
 Fixed X: O2(0.29315) H2C(0.267449) H2D(0.3244)
 Fixed Y: O2(0.60807) H2C(0.614321) H2D(0.629741)
 Fixed Z: O2(0.347341) H2C(0.33311) H2D(0.328641)
3.a Rotating group:
 O1(H1A,H1B)
3.b Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C25(H25)
3.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B)
3.d Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20)
3.e Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C)
;
_shelx_res_checksum              16576
_olex2_submission_special_instructions 'No special instructions were received'