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_7708859
_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         'C6 H18 F4 Ge P2'
_chemical_formula_sum            'C6 H18 F4 Ge P2'
_chemical_formula_weight         300.764
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_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                 91.210(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.1467(2)
_cell_length_b                   10.1678(4)
_cell_length_c                   9.5754(3)
_cell_measurement_reflns_used    2803
_cell_measurement_temperature    100.00(14)
_cell_measurement_theta_max      28.9320
_cell_measurement_theta_min      3.8270
_cell_volume                     598.31(4)
_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  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9575
_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    -70.00  65.00   1.00    1.00    --  -24.40  60.00 -60.00  135
  2  \w   -114.00  27.00   1.00    1.00    --  -24.40 -38.00  30.00  141
  3  \w   -114.00  21.00   1.00    1.00    --  -24.40 -57.00  90.00  135
  4  \w    -70.00  22.00   1.00    1.00    --  -24.40  60.00 150.00   92
  5  \w   -114.00  65.00   1.00    1.00    --  -24.40   0.00-180.00  179
;
_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      0.0310735000
_diffrn_orient_matrix_UB_12      0.0526473000
_diffrn_orient_matrix_UB_13      -0.0436683000
_diffrn_orient_matrix_UB_21      -0.0322029000
_diffrn_orient_matrix_UB_22      -0.0371678000
_diffrn_orient_matrix_UB_23      -0.0597446000
_diffrn_orient_matrix_UB_31      -0.1065087000
_diffrn_orient_matrix_UB_32      0.0265435000
_diffrn_orient_matrix_UB_33      0.0036035000
_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  0.0327
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 0.9575
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6990
_diffrn_reflns_point_group_measured_fraction_full 1.0000
_diffrn_reflns_point_group_measured_fraction_max 0.9575
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         28.90
_diffrn_reflns_theta_min         2.92
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.838
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82307
_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    1.669
_exptl_crystal_description       irregular
_exptl_crystal_F_000             305.010
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.7642
_refine_diff_density_min         -0.5345
_refine_diff_density_rms         0.1235
_refine_ls_d_res_high            0.7353
_refine_ls_d_res_low             6.9700
_refine_ls_goodness_of_fit_ref   1.0364
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    12
_refine_ls_number_parameters     64
_refine_ls_number_reflns         1509
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0364
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0304
_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^)+(0.0338P)^2^+0.8864P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0686
_refine_ls_wR_factor_ref         0.0736
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              6
_reflns_limit_h_min              -8
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              12
_reflns_limit_l_min              -6
_reflns_number_gt                1352
_reflns_number_total             1509
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1dt03339e2.cif
_cod_data_source_block           GeF4(PMe3)2-2
_cod_database_code               7708859
_chemical_oxdiff_formula         'Ge F4 P2 C6 H18'
_olex2_refinement_description
;
1.a Idealised Me refined as rotating group:
 C3(H3a,H3b,H3c), C2(H2a,H2b,H2c), C1(H1a,H1b,H1c)
;
_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 2.203
_oxdiff_exptl_absorpt_empirical_full_min 0.520