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_7708864
_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         'C12 H16 F6 Ge O6 P2 S2, 0.333(C1 H2 Cl2)'
_chemical_formula_sum            'C12.333 H16.667 Cl0.667 F6 Ge O6 P2 S2'
_chemical_formula_weight         597.210
_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                64.833(3)
_cell_angle_beta                 70.313(3)
_cell_angle_gamma                71.230(3)
_cell_formula_units_Z            2
_cell_length_a                   8.5322(2)
_cell_length_b                   12.5345(4)
_cell_length_c                   12.6057(4)
_cell_measurement_reflns_used    14812
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.1200
_cell_measurement_theta_min      1.8320
_cell_volume                     1123.35(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.8595
_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    -98.00  23.00   0.50   10.00    --   -9.10 -60.00 -30.00  242
  2  \w    -98.00  23.00   0.50   10.00    --   -9.10 -60.00  90.00  242
  3  \w    -98.00  22.00   0.50   10.00    --   -9.10 -57.00-180.00  240
  4  \w    -98.00  80.00   0.50   10.00    --   -9.10   0.00 -60.00  356
  5  \w    -44.00  54.00   0.50   10.00    --   -9.10  38.00 -30.00  196
  6  \w    -41.00  80.00   0.50   10.00    --   -9.10  60.00  60.00  242
;
_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      -0.0301603000
_diffrn_orient_matrix_UB_12      -0.0411809000
_diffrn_orient_matrix_UB_13      -0.0092455000
_diffrn_orient_matrix_UB_21      0.0143604000
_diffrn_orient_matrix_UB_22      -0.0438276000
_diffrn_orient_matrix_UB_23      0.0562202000
_diffrn_orient_matrix_UB_31      -0.0838900000
_diffrn_orient_matrix_UB_32      0.0217200000
_diffrn_orient_matrix_UB_33      0.0290128000
_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  0.0529
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 0.8595
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30424
_diffrn_reflns_point_group_measured_fraction_full 1.0000
_diffrn_reflns_point_group_measured_fraction_max 0.8595
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         32.63
_diffrn_reflns_theta_min         1.84
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.847
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.109a (Rigaku Oxford Diffraction, 2021)
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    1.766
_exptl_crystal_description       plate
_exptl_crystal_F_000             597.902
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.1003
_refine_diff_density_min         -1.2821
_refine_diff_density_rms         0.1414
_refine_ls_d_res_high            0.6590
_refine_ls_d_res_low             11.0938
_refine_ls_goodness_of_fit_ref   1.0350
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    28
_refine_ls_number_parameters     318
_refine_ls_number_reflns         7059
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0350
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.0010
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0266P)^2^+1.7319P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0842
_refine_ls_wR_factor_ref         0.0879
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -11
_reflns_limit_k_max              18
_reflns_limit_k_min              -16
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                6103
_reflns_number_total             7059
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1dt03339e2.cif
_cod_data_source_block           RKGeF3(diphos)OTf_auto
_cod_database_code               7708864
_chemical_oxdiff_formula         'Ge F6 S O3 P2 C20 H20'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(F2a)=Sof(F1a)=Sof(F3a)=1-FVAR(1)
 Sof(F3)=Sof(F1)=Sof(F2)=FVAR(1)
 Fixed Sof: Cl2(0.333335) Cl1(0.33333) C13(0.33333) H13a(0.33333) H13b(0.33333)
3.a Secondary CH2 refined with riding coordinates:
 C13(H13a,H13b)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C9(H9), C8(H8), C7(H7)
3.c Idealised Me refined as rotating group:
 C3(H3a,H3b,H3c), C1(H1a,H1b,H1c), C2(H2a,H2b,H2c), C4(H4a,H4b,H4c)
;
_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 3.680
_oxdiff_exptl_absorpt_empirical_full_min 0.194