Isolation of a Ge(I) Diradicaloid and Dihydrogen Splitting.
Sharma, Mahendra K.; Ebeler, Falk; Glodde, Timo; Neumann, Beate; Stammler, Hans-Georg; Ghadwal, Rajendra S.; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c11828

data_4135436
_publ_section_title
;
 Isolation of a Ge(I) Diradicaloid and Dihydrogen Splitting.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c11828
_journal_year                    2020
_chemical_formula_moiety         'C78 H88 Ge2 N4 Te2, 2(C6 H6)'
_chemical_formula_sum            'C90 H100 Ge2 N4 Te2'
_chemical_formula_weight         1638.11
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-02
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.2191(4)
_cell_length_b                   23.9973(5)
_cell_length_c                   27.2389(5)
_cell_measurement_reflns_used    31888
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      31.5000
_cell_measurement_theta_min      1.8540
_cell_volume                     15831.1(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.942
_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    -74.00 -49.00   1.00  191.00    --  -23.50-178.00 150.00   25
  2  \w     -4.00  22.00   1.00  191.00    --  -23.50  57.00 -90.00   26
  3  \w    -51.00 -25.00   1.00  191.00    --  -23.50 -57.00 120.00   26
  4  \w    -91.00 -65.00   1.00  191.00    --  -23.50 -57.00-180.00   26
  5  \w     -4.00  42.00   1.00  191.00    --   24.86  77.00-180.00   46
  6  \w    -46.00  47.00   1.00  191.00    --   24.86 -38.00-180.00   93
  7  \w      5.00  32.00   1.00  191.00    --   24.86  77.00-120.00   27
  8  \w     -7.00  65.00   1.00  191.00    --   24.86 -99.00  60.00   72
  9  \w     40.00  90.00   1.00  191.00    --   24.86  38.00 120.00   50
 10  \w    -46.00  32.00   1.00  191.00    --   24.86 -38.00 -60.00   78
 11  \w     -4.00  36.00   1.00  191.00    --   24.86  77.00 -30.00   40
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0040705000
_diffrn_orient_matrix_UB_12      0.0291535000
_diffrn_orient_matrix_UB_13      0.0022068000
_diffrn_orient_matrix_UB_21      0.0212064000
_diffrn_orient_matrix_UB_22      -0.0012667000
_diffrn_orient_matrix_UB_23      -0.0179299000
_diffrn_orient_matrix_UB_31      -0.0197887000
_diffrn_orient_matrix_UB_32      0.0046445000
_diffrn_orient_matrix_UB_33      -0.0187625000
_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  0.0758
_diffrn_reflns_av_unetI/netI     0.0573
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            194842
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.222
_diffrn_reflns_theta_min         1.682
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.529
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.824
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_description       plate
_exptl_crystal_F_000             6688
_exptl_crystal_size_max          0.381
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.808
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     899
_refine_ls_number_reflns         26402
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0246P)^2^+15.2116P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0815
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19042
_reflns_number_total             26402
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c11828_si_005.cif
_cod_data_source_block           compound6
_cod_database_code               4135436
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         ' C90H100Ge2N4Te2'
_diffrn_oxdiff_digest_frames
;
01293f98b49f47e8d7d3e85256c3e8af4e00513deaa
;
_diffrn_oxdiff_digest_hkl
;
01d9cb49acb728e1f6e1e7fbd8dd3c595619d8
;
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_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 Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C25(H25), C43(H43), C46(H46), C55(H55), C58(H58)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20), C29(H29), C30(H30),
 C31(H31), C32(H32), C33(H33), C39(H39), C40(H40), C41(H41), C51(H51), C52(H52),
  C53(H53), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C68(H68),
 C69(H69), C70(H70), C71(H71), C72(H72), C74(H74), C75(H75), C76(H76), C77(H77),
  C78(H78), C79(H79), C80(H80), C81(H81), C82(H82), C83(H83), C84(H84),
 C85(H85), C86(H86), C87(H87), C88(H88), C89(H89), C90(H90)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C59(H59A,H59B,
 H59C), C60(H60A,H60B,H60C)
;
_shelx_res_checksum              36186
_shelx_hkl_checksum              54570
_olex2_date_sample_data_collection 2020-02-27
_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 1.170
_oxdiff_exptl_absorpt_empirical_full_min 0.898