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_4135437
_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 S2, 1.5(C6 H6)'
_chemical_formula_sum            'C87 H97 Ge2 N4 S2'
_chemical_formula_weight         1407.98
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-04
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_cell_angle_alpha                101.491(3)
_cell_angle_beta                 101.127(2)
_cell_angle_gamma                100.578(2)
_cell_formula_units_Z            2
_cell_length_a                   11.0725(3)
_cell_length_b                   16.4856(6)
_cell_length_c                   22.3612(7)
_cell_measurement_reflns_used    13705
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      31.4750
_cell_measurement_theta_min      2.2100
_cell_volume                     3818.7(2)
_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      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.885
_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     -4.00  40.00   1.00   72.00    --   24.86  77.00 120.00   44
  2  \w     36.00  89.00   1.00   72.00    --   24.86  57.00  90.00   53
  3  \w     -4.00  41.00   1.00   72.00    --   24.86  77.00 -30.00   45
  4  \w    -40.00  43.00   1.00   72.00    --   24.86 -57.00-150.00   83
  5  \w    -45.00  40.00   1.00   72.00    --   24.86 -38.00  90.00   85
  6  \w      3.00  37.00   1.00   72.00    --   24.86  77.00-150.00   34
  7  \w    -42.00  53.00   1.00   72.00    --   24.86 -77.00   0.00   95
  8  \w    -29.00  -3.00   1.00   72.00    --   24.86 -38.00 -60.00   26
;
_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      0.0103169000
_diffrn_orient_matrix_UB_12      0.0308196000
_diffrn_orient_matrix_UB_13      -0.0176566000
_diffrn_orient_matrix_UB_21      -0.0656227000
_diffrn_orient_matrix_UB_22      -0.0103244000
_diffrn_orient_matrix_UB_23      -0.0144059000
_diffrn_orient_matrix_UB_31      -0.0094674000
_diffrn_orient_matrix_UB_32      0.0313018000
_diffrn_orient_matrix_UB_33      0.0243215000
_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  0.0313
_diffrn_reflns_av_unetI/netI     0.0603
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.885
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            44605
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.267
_diffrn_reflns_theta_min         1.788
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.888
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.488
_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    1.225
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1486
_exptl_crystal_size_max          0.436
_exptl_crystal_size_mid          0.171
_exptl_crystal_size_min          0.068
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     872
_refine_ls_number_reflns         24015
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0460
_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^)+(0.0267P)^2^+3.0456P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.1006
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18216
_reflns_number_total             24015
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c11828_si_004.cif
_cod_data_source_block           compound4
_cod_database_code               4135437
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C87H97Ge2N4S2
_shelx_estimated_absorpt_t_max   0.942
_shelx_estimated_absorpt_t_min   0.698
_diffrn_oxdiff_digest_frames
;
016a4f04332918792ff8fe65567d69406d00469aca4
;
_diffrn_oxdiff_digest_hkl
;
011fb90f7f0725345c7768ffb0ed66cd5a0231
;
_reflns_odcompleteness_completeness 99.90
_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:
 C12(H12), C15(H15), C24(H24), C27(H27), C43(H43), C46(H46), C55(H55), C58(H58)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C31(H31), C32(H32),
 C33(H33), C34(H34), C35(H35), 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)
2.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C), 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              64226
_shelx_hkl_checksum              45344
_olex2_date_sample_data_collection 2020-03-03
_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 1.231
_oxdiff_exptl_absorpt_empirical_full_min 0.808