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_7708857
_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         'C27 H24 F6 Ge O3 P2 S, C H2 Cl2'
_chemical_formula_sum            'C28 H26 Cl2 F6 Ge O3 P2 S'
_chemical_formula_weight         761.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_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
_cell_angle_beta                 94.8064(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.22780(19)
_cell_length_b                   12.3841(2)
_cell_length_c                   12.2598(2)
_cell_measurement_reflns_used    9316
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.7400
_cell_measurement_theta_min      3.1490
_cell_volume                     1547.39(5)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.939
_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    4.50    --  -15.60 -60.00 120.00  122
  2  \w    -44.00  74.00   1.00    4.50    --  -15.60  38.00 -60.00  118
  3  \w   -105.00  30.00   1.00    4.50    --  -15.60 -19.00-120.00  135
  4  \w    -48.00  48.00   1.00    4.50    --  -15.60  60.00  60.00   96
;
_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      -0.0071473000
_diffrn_orient_matrix_UB_12      0.0567392000
_diffrn_orient_matrix_UB_13      -0.0055348000
_diffrn_orient_matrix_UB_21      -0.0022849000
_diffrn_orient_matrix_UB_22      0.0047835000
_diffrn_orient_matrix_UB_23      0.0574628000
_diffrn_orient_matrix_UB_31      0.0692021000
_diffrn_orient_matrix_UB_32      0.0060554000
_diffrn_orient_matrix_UB_33      0.0062276000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0659
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21335
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.873
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.974
_diffrn_reflns_theta_min         2.987
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.400
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93093
_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    1.635
_exptl_crystal_description       block
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details
;
 Flack x determined using 2895 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.010(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         8585
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0238P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0688
_reflns_Friedel_coverage         0.857
_reflns_Friedel_fraction_full    0.977
_reflns_Friedel_fraction_max     0.808
_reflns_number_gt                7500
_reflns_number_total             8585
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03339e2.cif
_cod_data_source_block           gef3dppeotf-2
_cod_database_code               7708857
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Ge F6 O3 S P2 C27 H24'
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.873
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C27(H27A,H27B)
2.b Aromatic/amide H refined with riding coordinates:
 C25(H25), C26(H26), C6(H6), C11(H11), C10(H10), C16(H16), C20(H20), C23(H23),
 C3(H3), C24(H24), C12(H12), C9(H9), C22(H22), C4(H4), C5(H5), C19(H19),
 C18(H18), C17(H17), C8(H8), C2(H2)
;
_shelx_res_checksum              53832
_shelx_hkl_checksum              4334
_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 2.654
_oxdiff_exptl_absorpt_empirical_full_min 0.533