Low Oxidation State Silicon Clusters ‒ Synthesis and Structure of [NHCDippCu(η4-Si9)]3-
Geitner, Felix; Fässler, Thomas F; Chemical Communications  (2017) –; doi:10.1039/C7CC07995H

data_7120868
_publ_section_title
;
 Low Oxidation State Silicon Clusters -- Synthesis and Structure of
 [NHCDippCu(\h4-Si9)]3-
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C7CC07995H
_journal_year                    2017
_chemical_formula_moiety
'2(C27 H36 Cu N2 Si9), 3(C18 H36 K N2 O6), 26(H3 N), 3 (K)'
_chemical_formula_sum            'C108 H258 Cu2 K6 N36 O18 Si18'
_chemical_formula_weight         3216.79
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-08-03 deposited with the CCDC.
2017-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                87.0760(10)
_cell_angle_beta                 81.339(2)
_cell_angle_gamma                65.383(2)
_cell_formula_units_Z            2
_cell_length_a                   17.1066(3)
_cell_length_b                   18.1573(3)
_cell_length_c                   30.8056(5)
_cell_measurement_reflns_used    57166
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30.5291
_cell_measurement_theta_min      2.6314
_cell_volume                     8598.9(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 0.984
_diffrn_measured_fraction_theta_max 0.980
_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  0.0780
_diffrn_reflns_av_unetI/netI     0.0860
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            238718
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.636
_exptl_absorpt_coefficient_mu    0.580
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87454
_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            red
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_description       block
_exptl_crystal_F_000             3452
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: ammonia'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.988
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.900
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1709
_refine_ls_number_reflns         33153
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0543P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.1036
_reflns_number_gt                20085
_reflns_number_total             33153
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc07995h2.cif
_cod_data_source_block           FSG-270
_cod_database_code               7120868
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              40062