Alkali-metal-mediated zincation (AMMZn) meets N-heterocyclic carbene (NHC) chemistry: Zn‒H exchange reactions and structural authentication of a dinuclear Au(i) complex with a NHC anion
Armstrong, David R.; Baillie, Sharon E.; Blair, Victoria L.; Chabloz, Nicolas G.; Diez, Josefina; Garcia-Alvarez, Joaquin; Kennedy, Alan R.; Robertson, Stuart D.; Hevia, Eva; Chemical Science 4 (2013) 4259–; doi:10.1039/c3sc52101j

data_1514738
_publ_section_title
;
 Alkali-metal-mediated zincation (AMMZn) meets N-heterocyclic carbene
 (NHC) chemistry: Zn--H exchange reactions and structural authentication
 of a dinuclear Au(i) complex with a NHC anion
;
_journal_issue                   11
_journal_name_full               'Chemical Science'
_journal_page_first              4259
_journal_paper_doi               10.1039/c3sc52101j
_journal_volume                  4
_journal_year                    2013
_chemical_formula_sum            'C47 H77 N2 Na O3 Zn'
_chemical_formula_weight         806.47
_chemical_name_systematic
;
?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.9480(6)
_cell_length_b                   15.8780(8)
_cell_length_c                   24.9404(11)
_cell_measurement_reflns_used    8572
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.8594
_cell_measurement_theta_min      3.0356
_cell_volume                     4731.5(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'OD Xcalibur, Eos'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_sigmaI/netI    0.0883
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            30717
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    0.567
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67848
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.132
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.143(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         10854
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0928
_refine_ls_R_factor_gt           0.0557
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+1.8399P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.1010
_reflns_number_gt                7909
_reflns_number_total             10854
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c3sc52101j.txt
_cod_data_source_block           vb15
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               1514738