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_7703995
_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         'C22 H39 K O6, 2(H3 N)'
_chemical_formula_sum            'C22 H45 K N2 O6'
_chemical_formula_weight         472.70
_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     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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.1910(2)
_cell_length_b                   16.1458(3)
_cell_length_c                   32.8773(9)
_cell_measurement_reflns_used    188962
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.53
_cell_measurement_theta_min      2.67
_cell_volume                     5409.7(2)
_computing_cell_refinement       'STOE X-AREA 1.76'
_computing_data_collection       'STOE X-AREA 1.76'
_computing_data_reduction        'STOE X-AREA 1.76'
_computing_molecular_graphics    'DIAMOND 3.2k'
_computing_structure_refinement  SHELXL-2014/7
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'STOE StadiVari'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0115
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            148069
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         3.007
_diffrn_source                   'Genix 3D HF Mo'
_exptl_absorpt_coefficient_mu    0.231
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.977
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'STOE X-AREA 1.76'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2064
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Ammonia'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         5311
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0511P)^2^+2.1500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.0987
_reflns_number_gt                4543
_reflns_number_total             5311
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01096k2.cif
_cod_data_source_block           CW-34
_cod_depositor_comments
'Adding full bibliography for 7703988--7703995.cif.'
_cod_database_code               7703995
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              70614