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_7708862
_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         'C7 H18 F6 Ge O3 P2 S'
_chemical_formula_sum            'C7 H18 F6 Ge O3 P2 S'
_chemical_formula_weight         430.836
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_Int_Tables_number      61
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-26
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.3324(1)
_cell_length_b                   11.7241(1)
_cell_length_c                   23.5687(3)
_cell_measurement_reflns_used    47212
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      32.8360
_cell_measurement_theta_min      2.4980
_cell_volume                     3131.39(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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
_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 0.9149
_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    -26.00  94.00   0.50    5.24    --    5.00  57.00   0.00  240
  2  \w    -99.00  21.00   0.50    5.24    --   -9.90 -57.00   0.00  240
  3  \w    -99.00  22.00   0.50    5.24    --   -9.90 -60.00-150.00  242
  4  \w    -99.00  25.00   0.50    5.24    --   -9.90 -38.00 150.00  248
  5  \w    -99.00  22.00   0.50    5.24    --   -9.90 -60.00  90.00  242
  6  \w    -99.00  51.00   0.50    5.24    --   -9.90 -19.00-180.00  300
  7  \w    -71.00 -46.00   0.50    5.24    --   -9.90  19.00 -60.00   50
;
_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      -0.0092267000
_diffrn_orient_matrix_UB_12      -0.0023033000
_diffrn_orient_matrix_UB_13      0.0297513000
_diffrn_orient_matrix_UB_21      0.0127247000
_diffrn_orient_matrix_UB_22      0.0590801000
_diffrn_orient_matrix_UB_23      0.0020423000
_diffrn_orient_matrix_UB_31      -0.0605990000
_diffrn_orient_matrix_UB_32      0.0126982000
_diffrn_orient_matrix_UB_33      -0.0040969000
_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  0.0407
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_Laue_measured_fraction_full 0.9996
_diffrn_reflns_Laue_measured_fraction_max 0.9149
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            80977
_diffrn_reflns_point_group_measured_fraction_full 0.9996
_diffrn_reflns_point_group_measured_fraction_max 0.9149
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         32.59
_diffrn_reflns_theta_min         2.49
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.359
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81549
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.828
_exptl_crystal_description       block
_exptl_crystal_F_000             1733.595
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.8122
_refine_diff_density_min         -0.8203
_refine_diff_density_rms         0.0943
_refine_ls_d_res_high            0.6598
_refine_ls_d_res_low             8.1683
_refine_ls_goodness_of_fit_ref   1.0600
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    24
_refine_ls_number_parameters     187
_refine_ls_number_reflns         5222
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0600
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0207
_refine_ls_shift/su_max          -0.0009
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0223P)^2^+1.5402P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0486
_refine_ls_wR_factor_ref         0.0502
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              16
_reflns_limit_h_min              0
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              35
_reflns_limit_l_min              0
_reflns_number_gt                4649
_reflns_number_total             5222
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1dt03339e2.cif
_cod_data_source_block           RKGeF3(PMe3)2(OTF)
_cod_database_code               7708862
_chemical_oxdiff_formula         C7H18F6GeO3P2S
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C6(H6a,H6b,H6c), C4(H4a,H4b,H4c), C5(H5a,H5b,H5c), C3(H3a,H3b,H3c), C1(H1a,
 H1b,H1c), C2(H2a,H2b,H2c)
;
_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 3.167
_oxdiff_exptl_absorpt_empirical_full_min 0.461