Intermediates and products of the reaction of Zn(ii) organyls with tetrel element Zintl ions: cluster extension versus complexation.
Wallach, C.; Mayer, K.; Henneberger, T.; Klein, W.; Fässler, T F; Dalton transactions (Cambridge, England : 2003) 49 (2020) 6191–6198; doi:10.1039/d0dt01096k

data_7703992
_publ_section_title
;
 Intermediates and products of the reaction of Zn(ii) organyls with tetrel
 element Zintl ions: cluster extension versus complexation.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6191
_journal_page_last               6198
_journal_paper_doi               10.1039/d0dt01096k
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C27 H33 Zn, C16 H35 K N O7, C4 H8 O'
_chemical_formula_sum            'C47 H76 K N O8 Zn'
_chemical_formula_weight         887.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-02-05 deposited with the CCDC.	2020-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.486(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7570(5)
_cell_length_b                   13.1722(5)
_cell_length_c                   23.6712(8)
_cell_measurement_reflns_used    11308
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.9070
_cell_measurement_theta_min      2.6645
_cell_volume                     4898.0(3)
_computing_cell_refinement
; 
 CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.34d 
;
_computing_data_collection
; 
 CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.33.34d 
;
_computing_data_reduction
; 
 CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.34d 
;
_computing_molecular_graphics    'DIAMOND 3.2k'
_computing_structure_refinement  SHELXL-2014/7
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 16.0238
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Oxford Xcalibur 3'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0706
_diffrn_reflns_av_unetI/netI     0.1068
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            55312
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.721
_exptl_absorpt_coefficient_mu    0.635
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82228
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.34d 
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_description       plate
_exptl_crystal_F_000             1912
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Ammonia'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.659
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.840
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         9472
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.840
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0555P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1018
_refine_ls_wR_factor_ref         0.1107
_reflns_number_gt                4880
_reflns_number_total             9472
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01096k2.cif
_cod_data_source_block           TH464
_cod_depositor_comments
'Adding full bibliography for 7703988--7703995.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7703992
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              46171