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_7703994
_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         '2(C12 H30 K N2 O6), C8 H36 N8 Zn5, H3 N'
_chemical_formula_sum            'C32 H99 K2 N13 O12 Zn5'
_chemical_formula_weight         1263.29
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                89.02(3)
_cell_angle_beta                 77.37(3)
_cell_angle_gamma                87.11(3)
_cell_formula_units_Z            2
_cell_length_a                   11.554(2)
_cell_length_b                   14.140(3)
_cell_length_c                   18.988(4)
_cell_measurement_reflns_used    177980
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      34.015
_cell_measurement_theta_min      3.345
_cell_volume                     3023.2(11)
_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                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'STOE StadiVari'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0192
_diffrn_reflns_av_unetI/netI     0.0114
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            69261
_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         25.998
_diffrn_reflns_theta_min         3.423
_diffrn_source                   'Genix 3D HF Mo'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.148
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.875
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'STOE X-AREA 1.76'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_description       column
_exptl_crystal_F_000             1332
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Ammonia'
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.768
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         11852
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0267
_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^)+(0.0237P)^2^+3.0835P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0613
_refine_ls_wR_factor_ref         0.0668
_reflns_number_gt                10537
_reflns_number_total             11852
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01096k2.cif
_cod_data_source_block           KM-668
_cod_depositor_comments
'Adding full bibliography for 7703988--7703995.cif.'
_cod_database_code               7703994
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              50744