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_7708856
_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_absolute_configuration ad
_chemical_formula_moiety         'C12 H16 F8 Ge O6 P2 S2'
_chemical_formula_sum            'C12 H16 F8 Ge O6 P2 S2'
_chemical_formula_weight         606.90
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-09-30 deposited with the CCDC.	2021-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   8.49904(14)
_cell_length_b                   15.8315(3)
_cell_length_c                   16.3349(4)
_cell_measurement_reflns_used    28410
_cell_measurement_temperature    100.2(8)
_cell_measurement_theta_max      30.5370
_cell_measurement_theta_min      3.4470
_cell_volume                     2197.90(8)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.2(8)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.977
_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  74.00   1.00    5.00    --  -15.70   0.00  30.00  179
  2  \w   -105.00  17.00   1.00    5.00    --  -15.70 -60.00-150.00  122
  3  \w   -105.00  17.00   1.00    5.00    --  -15.70 -60.00  30.00  122
  4  \w   -105.00  17.00   1.00    5.00    --  -15.70 -60.00 150.00  122
  5  \w   -105.00  17.00   1.00    5.00    --  -15.70 -60.00 -60.00  122
  6  \w    -48.00  74.00   1.00    5.00    --  -15.70  60.00  60.00  122
  7  \w    -48.00  74.00   1.00    5.00    --  -15.70  60.00 -60.00  122
  8  \w    -48.00  16.00   1.00    5.00    --  -15.70  57.00 120.00   64
  9  \w    -48.00  74.00   1.00    5.00    --  -15.70  60.00-180.00  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      -0.0120724000
_diffrn_orient_matrix_UB_12      0.0021531000
_diffrn_orient_matrix_UB_13      -0.0429180000
_diffrn_orient_matrix_UB_21      -0.0820126000
_diffrn_orient_matrix_UB_22      -0.0056101000
_diffrn_orient_matrix_UB_23      0.0060039000
_diffrn_orient_matrix_UB_31      -0.0097587000
_diffrn_orient_matrix_UB_32      0.0443893000
_diffrn_orient_matrix_UB_33      0.0027882000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0710
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            71065
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.124
_diffrn_reflns_theta_min         2.993
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.832
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94884
_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_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.834
_exptl_crystal_description       needle
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.767
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.134
_refine_ls_abs_structure_details
;
 Flack x determined using 2345 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.011(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         6832
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0612
_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^)+(0.0540P)^2^+7.9413P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1425
_refine_ls_wR_factor_ref         0.1455
_reflns_Friedel_coverage         0.762
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.949
_reflns_number_gt                6280
_reflns_number_total             6832
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03339e2.cif
_cod_data_source_block           rk[gef2(diphos)][otf]2
_cod_database_code               7708856
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Ge F8 P2 C15 H15 S2 O6'
_chemical_oxdiff_usercomment     'colourless chunk - '
_cell_oxdiff_angle_alpha         89.9329(17)
_cell_oxdiff_angle_beta          89.9770(14)
_cell_oxdiff_angle_gamma         90.0142(13)
_cell_oxdiff_length_a            8.49779(11)
_cell_oxdiff_length_b            15.8347(3)
_cell_oxdiff_length_c            16.3340(4)
_cell_oxdiff_measurement_reflns_used 28408
_cell_oxdiff_volume              2197.90(7)
_shelx_estimated_absorpt_t_max   0.898
_shelx_estimated_absorpt_t_min   0.611
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C6(H6), C8(H8), C7(H7)
2.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              15131
_shelx_hkl_checksum              95625
_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 1.595
_oxdiff_exptl_absorpt_empirical_full_min 0.633