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_4135438
_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         '2(C33 H39 Ge N2), C4 H8 O'
_chemical_formula_sum            'C70 H86 Ge2 N4 O'
_chemical_formula_weight         1144.60
_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     direct
_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                82.394(3)
_cell_angle_beta                 84.112(3)
_cell_angle_gamma                87.309(3)
_cell_formula_units_Z            2
_cell_length_a                   12.8343(4)
_cell_length_b                   14.2908(5)
_cell_length_c                   17.1398(6)
_cell_measurement_reflns_used    10624
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.9800
_cell_measurement_theta_min      3.1170
_cell_volume                     3097.78(18)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.975
_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   -124.00  47.00   1.00   55.50    --  -38.50   0.00   0.00  171
  2  \w    -50.00  11.00   1.00   55.50    --  -38.50  38.00  30.00   61
  3  \w     30.00  87.00   1.00   55.50    --   42.70-125.00 -60.00   57
  4  \w     10.00  44.00   1.00   55.50    --   42.70 -99.00-180.00   34
  5  \w     32.00  90.00   1.00   55.50    --   42.70-125.00 120.00   58
  6  \w    138.00 169.00   1.00  150.00    --  111.00  61.00  90.00   31
  7  \w     85.00 123.00   1.00  150.00    --  111.00  61.00  90.00   38
  8  \w    104.00 174.00   1.00  150.00    --  111.00  77.00 120.00   70
  9  \w     51.00 132.00   1.00  150.00    --  111.00 -45.00 -60.00   81
 10  \w     42.00  85.00   1.00  150.00    --  111.00-125.00 150.00   43
 11  \w    132.00 159.00   1.00  150.00    --  111.00  77.00 -60.00   27
 12  \w     90.00 178.00   1.00  150.00    --  111.00  45.00 -90.00   88
 13  \w     60.00 107.00   1.00  150.00    --  111.00 -94.00   0.00   47
 14  \w    104.00 172.00   1.00  150.00    --  111.00  77.00   0.00   68
 15  \w    106.00 175.00   1.00  150.00    --  111.00  77.00 -30.00   69
 16  \w     47.00  78.00   1.00  150.00    --  111.00-125.00   0.00   31
 17  \w     68.00 134.00   1.00  150.00    --  111.00 -61.00 150.00   66
 18  \w     35.00 107.00   1.00  150.00    --  111.00 -94.00 -60.00   72
 19  \w     42.00 113.00   1.00  150.00    --  111.00-125.00-180.00   71
 20  \w     79.00 106.00   1.00  150.00    --  111.00-102.00 110.00   27
 21  \w     36.00 107.00   1.00  150.00    --  111.00 -94.00-180.00   71
 22  \w     65.00 107.00   1.00  150.00    --  111.00 -94.00  60.00   42
 23  \w    112.00 167.00   1.00  150.00    --  111.00  30.00  60.00   55
 24  \w     80.00 107.00   1.00  150.00    --  111.00 -94.00-120.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0033247000
_diffrn_orient_matrix_UB_12      -0.0563421000
_diffrn_orient_matrix_UB_13      0.0828542000
_diffrn_orient_matrix_UB_21      0.1040668000
_diffrn_orient_matrix_UB_22      -0.0489826000
_diffrn_orient_matrix_UB_23      -0.0279666000
_diffrn_orient_matrix_UB_31      0.0611340000
_diffrn_orient_matrix_UB_32      0.0791713000
_diffrn_orient_matrix_UB_33      0.0255847000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_unetI/netI     0.0469
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26968
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.452
_diffrn_reflns_theta_min         2.613
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.532
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.880
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.69a (Rigaku Oxford Diffraction, 2020)
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            'metallic black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_description       block
_exptl_crystal_F_000             1212
_exptl_crystal_size_max          0.146
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.081
_refine_diff_density_max         1.625
_refine_diff_density_min         -0.870
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     710
_refine_ls_number_reflns         12689
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0597P)^2^+1.8936P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1214
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10505
_reflns_number_total             12689
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c11828_si_003.cif
_cod_data_source_block           compound3
_cod_original_cell_volume        3097.78(19)
_cod_database_code               4135438
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C70H86Ge2N4O
_diffrn_oxdiff_digest_frames
;
016e82f087c570cbfd31b01814576e9570014650cb3
;
_diffrn_oxdiff_digest_hkl
;
010c09fa82bef31d43e90ca2b0f6764978ab89
;
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,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 Secondary CH2 refined with riding coordinates:
 C67(H67A,H67B), C68(H68A,H68B), C69(H69A,H69B), C70(H70A,H70B)
2.c 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)
2.d 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              75788
_shelx_hkl_checksum              73283
_olex2_date_sample_data_collection 2020-02-26
_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 1.681
_oxdiff_exptl_absorpt_empirical_full_min 0.330