Neutral and cationic germanium(IV) fluoride complexes with phosphine coordination – synthesis, spectroscopy and structures
King, Rhys; Levason, William; Reid, Gillian; Dalton Transactions  (2021) –; doi:10.1039/D1DT03339E

data_7708860
_publ_section_title
;
 Neutral and cationic germanium(IV) fluoride complexes with phosphine
 coordination -- synthesis, spectroscopy and structures
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03339E
_journal_year                    2021
_chemical_formula_moiety         'C14 H30 As2 Cl2 F6 Ge O6 S2'
_chemical_formula_sum            'C14 H30 As2 Cl2 F6 Ge O6 S2'
_chemical_formula_weight         765.83
_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
_audit_creation_date             2021-09-14
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396)
;
_audit_update_record
;
2021-09-30 deposited with the CCDC.	2021-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                104.887(3)
_cell_angle_beta                 101.440(3)
_cell_angle_gamma                97.269(3)
_cell_formula_units_Z            2
_cell_length_a                   9.6136(3)
_cell_length_b                   9.7490(4)
_cell_length_c                   15.2210(5)
_cell_measurement_reflns_used    10889
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      32.6400
_cell_measurement_theta_min      3.5760
_cell_volume                     1327.35(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -100.00 -63.00   1.00    1.42    --  -13.90 -38.00  90.00   37
  2  \w    -38.00 -12.00   1.00    1.42    --  -13.90 -38.00  90.00   26
  3  \w    -71.00  12.00   1.00    1.42    --  -13.90 -60.00  30.00   83
  4  \w   -103.00  -4.00   1.00    1.42    --  -13.90 -60.00-150.00   99
  5  \w    -82.00  11.00   1.00    1.42    --  -13.90 -60.00 -60.00   93
  6  \w    -26.00  48.00   1.00    1.42    --  -13.90  38.00-180.00   74
  7  \w     12.00  39.00   1.00    1.42    --  -13.90  19.00  60.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0280254000
_diffrn_orient_matrix_UB_12      0.0222925000
_diffrn_orient_matrix_UB_13      0.0492490000
_diffrn_orient_matrix_UB_21      0.0192397000
_diffrn_orient_matrix_UB_22      0.0721152000
_diffrn_orient_matrix_UB_23      -0.0010952000
_diffrn_orient_matrix_UB_31      -0.0686809000
_diffrn_orient_matrix_UB_32      0.0132757000
_diffrn_orient_matrix_UB_33      0.0064409000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_av_unetI/netI     0.0740
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22109
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.908
_diffrn_reflns_theta_min         2.897
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.057
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36618
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.61a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.916
_exptl_crystal_description       block
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.167
_refine_diff_density_min         -1.118
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         8925
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0290P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.0882
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7063
_reflns_number_total             8925
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03339e2.cif
_cod_data_source_block           gecl2(aset3)2otf2
_cod_original_cell_volume        1327.35(8)
_cod_database_code               7708860
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Ge Cl2 As2 O6 F6 S2 H30 C13'
_shelx_estimated_absorpt_t_max   0.823
_shelx_estimated_absorpt_t_min   0.498
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C1(H1A,H1B), C9(H9A,H9B), C3(H3A,H3B), C11(H11A,H11B), C5(H5A,H5B)
2.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C2(H2A,H2B,H2C), C6(H6A,H6B,H6C), C4(H4A,H4B,H4C),
 C8(H8A,H8B,H8C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              67223
_shelx_hkl_checksum              87401
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.857
_oxdiff_exptl_absorpt_empirical_full_min 0.368