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_7708863
_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         '3(C8 H18 F8 Ge O6 P2 S2)'
_chemical_formula_sum            'C24 H54 F24 Ge3 O18 P6 S6'
_chemical_formula_weight         1682.725
_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_Int_Tables_number      2
_audit_creation_date             2021-11-02
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396)
;
_audit_update_record
;
2021-11-05 deposited with the CCDC.	2021-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                93.050(3)
_cell_angle_beta                 94.382(3)
_cell_angle_gamma                91.974(3)
_cell_formula_units_Z            2
_cell_length_a                   9.3701(3)
_cell_length_b                   15.5931(6)
_cell_length_c                   21.5703(7)
_cell_measurement_reflns_used    15063
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.8660
_cell_measurement_theta_min      2.2810
_cell_volume                     3135.60(19)
_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  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.9996
_diffrn_measured_fraction_theta_max 0.8172
_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    -41.00  70.00   0.50    7.39    --   -8.40  36.00-137.00  222
  2  \w    -90.00  25.00   0.50    7.39    --   -8.40 -36.00  66.00  230
  3  \w    -91.00  15.00   0.50    7.39    --   -8.40 -60.00   0.00  212
  4  \w    -77.00 -50.00   0.50    7.39    --   -8.40 -60.00 150.00   54
  5  \w    -38.00  23.00   0.50    7.39    --   -8.40 -60.00 150.00  122
  6  \w    -74.00 -16.00   0.50    7.39    --   -8.40 -60.00 -60.00  116
  7  \w    -98.00 -61.00   0.50    7.39    --   -8.40 -57.00 -90.00   74
;
_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      0.0470927000
_diffrn_orient_matrix_UB_12      -0.0305409000
_diffrn_orient_matrix_UB_13      0.0124058000
_diffrn_orient_matrix_UB_21      0.0594385000
_diffrn_orient_matrix_UB_22      0.0246259000
_diffrn_orient_matrix_UB_23      -0.0088236000
_diffrn_orient_matrix_UB_31      0.0046727000
_diffrn_orient_matrix_UB_32      0.0232156000
_diffrn_orient_matrix_UB_33      0.0293140000
_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  0.0672
_diffrn_reflns_av_unetI/netI     0.0759
_diffrn_reflns_Laue_measured_fraction_full 0.9996
_diffrn_reflns_Laue_measured_fraction_max 0.8172
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            57396
_diffrn_reflns_point_group_measured_fraction_full 0.9996
_diffrn_reflns_point_group_measured_fraction_max 0.8172
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         32.86
_diffrn_reflns_theta_min         2.18
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.909
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60365
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1685.364
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.5245
_refine_diff_density_min         -1.3404
_refine_diff_density_rms         0.2479
_refine_ls_d_res_high            0.6550
_refine_ls_d_res_low             9.3357
_refine_ls_goodness_of_fit_ref   1.0256
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    74
_refine_ls_number_parameters     849
_refine_ls_number_reflns         19099
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0256
_refine_ls_R_factor_all          0.1134
_refine_ls_R_factor_gt           0.0709
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1357P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1898
_refine_ls_wR_factor_ref         0.2168
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              21
_reflns_limit_k_min              -21
_reflns_limit_l_max              31
_reflns_limit_l_min              0
_reflns_number_gt                12030
_reflns_number_total             19099
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1dt03339e2.cif
_cod_data_source_block           GeF2PMe32OTf24
_cod_database_code               7708863
_chemical_oxdiff_formula         'Ge F8 S2 O6 P2 C8 H18 '
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(S5a)=Sof(O15a)=Sof(O16a)=Sof(C12a)=Sof(F19a)=Sof(F21a)=Sof(F20a)=1-FVAR(1)
 Sof(O15)=Sof(S5)=Sof(F21)=Sof(O16)=Sof(C12)=Sof(F19)=Sof(F20)=FVAR(1)
 Sof(F12a)=Sof(C21a)=Sof(F11a)=Sof(F10a)=1-FVAR(2)
 Sof(F11)=Sof(F12)=Sof(F10)=Sof(C21)=FVAR(2)
3.a Idealised Me refined as rotating group:
 C8(H8a,H8b,H8c), C11(H11a,H11b,H11c), C16(H16a,H16b,H16c), C4(H4a,H4b,H4c),
 C2(H2a,H2b,H2c), C14(H14a,H14b,H14c), C19(H19a,H19b,H19c), C6(H6a,H6b,H6c),
 C3(H3a,H3b,H3c), C1(H1a,H1b,H1c), C17(H17a,H17b,H17c), C5(H5a,H5b,H5c), C7(H7a,
 H7b,H7c), C10(H10a,H10b,H10c), C9(H9a,H9b,H9c), C15(H15a,H15b,H15c), C13(H13a,
 H13b,H13c), C18(H18a,H18b,H18c)
;
_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 3.601
_oxdiff_exptl_absorpt_empirical_full_min 0.553