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_7708858
_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         'C41 H39 F4 Ge P3, C H2 Cl2'
_chemical_formula_sum            'C42 H41 Cl2 F4 Ge P3'
_chemical_formula_weight         858.15
_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'
_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                 96.8620(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9614(2)
_cell_length_b                   12.9040(2)
_cell_length_c                   21.6728(3)
_cell_measurement_reflns_used    21337
_cell_measurement_temperature    100
_cell_measurement_theta_max      33.5800
_cell_measurement_theta_min      1.8570
_cell_volume                     3876.56(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_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_temperature      100
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.869
_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    -63.00 -28.00   0.50    3.90    --  -12.70 -19.00-124.00   70
  2  \w    -21.00   5.00   0.50    3.90    --  -12.70  19.00  43.00   52
  3  \w    -44.00  47.00   0.50    3.90    --  -12.70  60.00 150.00  182
  4  \w      0.00  77.00   0.50    3.90    --  -12.70  57.00-150.00  154
  5  \w    -95.00  17.00   0.50    3.90    --  -12.70 -57.00 150.00  224
;
_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      0.0094460000
_diffrn_orient_matrix_UB_12      0.0104560000
_diffrn_orient_matrix_UB_13      -0.0308489000
_diffrn_orient_matrix_UB_21      0.0498844000
_diffrn_orient_matrix_UB_22      -0.0089555000
_diffrn_orient_matrix_UB_23      0.0088985000
_diffrn_orient_matrix_UB_31      -0.0065159000
_diffrn_orient_matrix_UB_32      -0.0531845000
_diffrn_orient_matrix_UB_33      -0.0074978000
_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  0.0289
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.869
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            48266
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.869
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.898
_diffrn_reflns_theta_min         1.893
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.102
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58737
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.69a (Rigaku Oxford Diffraction, 2020)
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    1.470
_exptl_crystal_description       block
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.851
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         13630
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+2.9161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0763
_refine_ls_wR_factor_ref         0.0805
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11082
_reflns_number_total             13630
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03339e2.cif
_cod_data_source_block           gef4(triphos)-2
_cod_database_code               7708858
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Ge F4 P3 C41 H39'
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.770
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C5(H5A,H5B), C4(H4A,H4B), C42(H42A,H42B)
1.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C7(H7), C10(H10), C31(H31), C25(H25), C9(H9), C35(H35), C17(H17),
 C13(H13), C37(H37), C19(H19), C29(H29), C23(H23), C8(H8), C21(H21), C38(H38),
 C41(H41), C26(H26), C15(H15), C16(H16), C32(H32), C28(H28), C22(H22), C14(H14),
  C27(H27), C33(H33), C39(H39), C34(H34), C40(H40), C20(H20)
1.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_shelx_res_checksum              4285
_shelx_hkl_checksum              46007
_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 1.492
_oxdiff_exptl_absorpt_empirical_full_min 0.560