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_7708861
_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         '4(C13 H16 F10 Ge O9 P2 S3), C0.6 H1.2 Cl1.2'
_chemical_formula_sum            'C52.6 H65.2 Cl1.2 F40 Ge4 O36 P8 S12'
_chemical_formula_weight         2998.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'I 2y'
_space_group_name_H-M_alt        'I 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                90
_cell_angle_beta                 100.2150(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.7401(2)
_cell_length_b                   9.08810(10)
_cell_length_c                   33.6730(3)
_cell_measurement_reflns_used    40734
_cell_measurement_temperature    100.1(4)
_cell_measurement_theta_max      30.7380
_cell_measurement_theta_min      1.9740
_cell_volume                     5342.84(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.1(4)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.952
_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   -105.00  17.00   1.00   13.19    --  -15.60 -60.00 -90.00  122
  2  \w   -105.00  17.00   1.00   13.19    --  -15.60 -60.00 150.00  122
  3  \w    -44.00  74.00   1.00   13.19    --  -15.60  38.00  90.00  118
  4  \w    -44.00  74.00   1.00   13.19    --  -15.60  38.00   0.00  118
  5  \w   -105.00  17.00   1.00   13.19    --  -15.60 -60.00  60.00  122
  6  \w   -105.00  13.00   1.00   13.19    --  -15.60 -38.00 120.00  118
  7  \w    -48.00  14.00   1.00   13.19    --  -15.60  60.00 -90.00   62
  8  \w    -48.00  74.00   1.00   13.19    --  -15.60  57.00-150.00  122
;
_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      -0.0330834000
_diffrn_orient_matrix_UB_12      0.0169187000
_diffrn_orient_matrix_UB_13      0.0082523000
_diffrn_orient_matrix_UB_21      -0.0232150000
_diffrn_orient_matrix_UB_22      -0.0105615000
_diffrn_orient_matrix_UB_23      -0.0192183000
_diffrn_orient_matrix_UB_31      -0.0041771000
_diffrn_orient_matrix_UB_32      -0.0754514000
_diffrn_orient_matrix_UB_33      0.0045424000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            72764
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.119
_diffrn_reflns_theta_min         1.999
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.642
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.864
_exptl_crystal_description       plate
_exptl_crystal_F_000             2978
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.570
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Flack x determined using 5930 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     707
_refine_ls_number_reflns         15790
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0321
_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^)+(0.0306P)^2^+3.8959P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0681
_reflns_Friedel_coverage         0.823
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.878
_reflns_number_gt                14581
_reflns_number_total             15790
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03339e2.cif
_cod_data_source_block           vgrkgefdiphosotf3abeam
_cod_original_formula_sum        'C52.60 H65.20 Cl1.20 F40 Ge4 O36 P8 S12'
_cod_database_code               7708861
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Ge F9 P2 C15 H20 S2 O6'
_chemical_oxdiff_usercomment     'Long rectangle'
_shelx_estimated_absorpt_t_max   0.952
_shelx_estimated_absorpt_t_min   0.853
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_olex2_refinement_description
;
1. Others
 Fixed Sof: Cl1(0.6) C27(0.3) H27A(0.3) H27B(0.3)
2.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C16(H16), C7(H7), C8(H8), C17(H17), C9(H9), C18(H18), C19(H19)
2.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C2(H2A,H2B,H2C), C1(H1A,H1B,H1C), C11(H11A,H11B,H11C),
 C14(H14A,H14B,H14C), C3(H3A,H3B,H3C), C13(H13A,H13B,H13C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              97179
_shelx_hkl_checksum              28592
_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 1.967
_oxdiff_exptl_absorpt_empirical_full_min 0.578