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_7708865
_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
'C27.7 H24 F7.4 Ge O5.1 P2 S1.7, 1.3(C H2 Cl2)'
_chemical_formula_sum            'C29 H26.6 Cl2.6 F7.4 Ge O5.1 P2 S1.7'
_chemical_formula_weight         878.50
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_atom_sites_solution_hydrogens   mixed
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5994(2)
_cell_length_b                   20.7200(4)
_cell_length_c                   14.7520(2)
_cell_measurement_reflns_used    28819
_cell_measurement_temperature    99.9(3)
_cell_measurement_theta_max      31.8840
_cell_measurement_theta_min      2.9540
_cell_volume                     3545.49(10)
_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  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(3)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.974
_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   -112.00  13.00   1.00   10.00    --  -22.70 -60.00 120.00  125
  2  \w   -112.00  13.00   1.00   10.00    --  -22.70 -60.00-120.00  125
  3  \w   -112.00  13.00   1.00   10.00    --  -22.70 -60.00 -30.00  125
  4  \w   -112.00  13.00   1.00   10.00    --  -22.70 -60.00  60.00  125
  5  \w   -112.00  13.00   1.00   10.00    --  -22.70 -60.00 -90.00  125
  6  \w    -58.00  67.00   1.00   10.00    --  -22.70  60.00-150.00  125
  7  \w    -58.00  67.00   1.00   10.00    --  -22.70  60.00-120.00  125
  8  \w    -57.00  66.00   1.00   10.00    --  -22.70  60.00 -60.00  123
  9  \w   -102.00  13.00   1.00   10.00    --  -22.70 -60.00   0.00  115
;
_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      -0.0015452000
_diffrn_orient_matrix_UB_12      -0.0342174000
_diffrn_orient_matrix_UB_13      -0.0015401000
_diffrn_orient_matrix_UB_21      -0.0601232000
_diffrn_orient_matrix_UB_22      0.0010449000
_diffrn_orient_matrix_UB_23      -0.0084217000
_diffrn_orient_matrix_UB_31      0.0107712000
_diffrn_orient_matrix_UB_32      0.0009283000
_diffrn_orient_matrix_UB_33      -0.0473339000
_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  0.0926
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            105333
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.457
_diffrn_reflns_theta_min         2.931
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.327
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49688
_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    1.646
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1766
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.777
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         6229
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0375P)^2^+3.2252P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1046
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5374
_reflns_number_total             6229
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03339e2.cif
_cod_data_source_block           gef3dppeotf
_cod_original_formula_sum        'C29 H26.60 Cl2.60 F7.40 Ge O5.10 P2 S1.70'
_cod_database_code               7708865
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Ge F6 O3 P2 S C29 H42'
_shelx_estimated_absorpt_t_max   0.925
_shelx_estimated_absorpt_t_min   0.879
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(Ge1) = Uanis(F6)
2. Others
 Sof(Cl2)=1-FVAR(1)
 Sof(Cl1)=FVAR(1)
 Fixed Sof: S1(0.85) O1(0.85) F4(0.85) F3(0.85) O3(0.85) F2(0.85) O2(0.85)
 C14(0.85) Cl3(0.15) Cl4(0.15) C16(0.15) H16A(0.15) H16B(0.15) F6(0.15)
3.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C16(H16A,H16B)
3.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C12(H12), C2(H2), C6(H6), C11(H11), C9(H9), C4(H4), C5(H5), C3(H3),
 C10(H10)
;
_shelx_res_checksum              35618
_shelx_hkl_checksum              89442
_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 3.605
_oxdiff_exptl_absorpt_empirical_full_min 0.429