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_4135439
_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         'C66 H78 Cl2 Ge2 N4, 2(C4 H8 O)'
_chemical_formula_sum            'C74 H94 Cl2 Ge2 N4 O2'
_chemical_formula_weight         1287.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-13
_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                 98.358(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7437(4)
_cell_length_b                   20.2913(4)
_cell_length_c                   24.8641(4)
_cell_measurement_reflns_used    40383
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      29.5630
_cell_measurement_theta_min      1.5060
_cell_volume                     6860.4(3)
_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      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.986
_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     17.00  94.00   1.00   45.00    --   24.79-148.00 -20.41   77
  2  \w     -4.00  42.00   1.00   45.00    --   24.79  77.00-120.00   46
  3  \w      3.00  95.00   1.00   45.00    --   24.79  38.00  30.00   92
  4  \w      6.00  93.00   1.00   45.00    --   24.79  57.00 -90.00   87
  5  \w     39.00  99.00   1.00   45.00    --   24.79 178.00-120.00   60
  6  \w    -44.00  43.00   1.00   45.00    --   24.79 -57.00 -30.00   87
  7  \w    -44.00  43.00   1.00   45.00    --   24.79 -57.00-150.00   87
  8  \w     -4.00  42.00   1.00   45.00    --   24.79  77.00   0.00   46
  9  \w    -46.00  96.00   1.00   45.00    --   24.79   0.00 -30.00  142
 10  \w    -46.00  47.00   1.00   45.00    --   24.79 -38.00-120.00   93
 11  \w      6.00  93.00   1.00   45.00    --   24.79  57.00 150.00   87
 12  \w      7.00  80.00   1.00   45.00    --   24.79-126.00-173.03   73
 13  \w      6.00  93.00   1.00   45.00    --   24.79  57.00  60.00   87
 14  \w      2.00  77.00   1.00   45.00    --   24.79-120.00  95.72   75
 15  \w    -95.00  48.00   1.00   45.00    --  -23.50   0.00-150.00  143
 16  \w    -95.00  48.00   1.00   45.00    --  -23.50   0.00-180.00  143
 17  \w    -95.00  48.00   1.00   45.00    --  -23.50   0.00-120.00  143
 18  \w    -97.00 -39.00   1.00   45.00    --  -23.50-178.00 -30.00   58
 19  \w    -15.00  65.00   1.00   45.00    --   24.79 -99.00   0.00   80
 20  \w     -4.00  42.00   1.00   45.00    --   24.79  77.00-180.00   46
 21  \w     -4.00   7.00   1.00   45.00    --   24.79  77.00 -90.00   11
;
_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      0.0497404000
_diffrn_orient_matrix_UB_12      0.0067803000
_diffrn_orient_matrix_UB_13      0.0105913000
_diffrn_orient_matrix_UB_21      0.0104125000
_diffrn_orient_matrix_UB_22      -0.0342458000
_diffrn_orient_matrix_UB_23      0.0006981000
_diffrn_orient_matrix_UB_31      0.0117673000
_diffrn_orient_matrix_UB_32      0.0017788000
_diffrn_orient_matrix_UB_33      -0.0268085000
_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  0.0987
_diffrn_reflns_av_unetI/netI     0.0738
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            172538
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         1.498
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.001
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.394
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_description       block
_exptl_crystal_F_000             2720
_exptl_crystal_size_max          0.304
_exptl_crystal_size_mid          0.225
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.021
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.080
_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     783
_refine_ls_number_reflns         13326
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0713P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1263
_refine_ls_wR_factor_ref         0.1325
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8674
_reflns_number_total             13326
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -175.9596\% 
 around [-0.00 1.00 0.01] (reciprocal) or [-0.01 1.00 0.01] (direct)
;
_cod_data_source_file            ja0c11828_si_002.cif
_cod_data_source_block           compound2
_cod_database_code               4135439
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C74H94Cl2Ge2N4O2
_shelx_estimated_absorpt_t_max   0.840
_shelx_estimated_absorpt_t_min   0.751
_diffrn_oxdiff_digest_frames
;
0121d3967fc7e636a1b558622b753c2f8901765393e
;
_diffrn_oxdiff_digest_hkl
;
012606e48db69e3d6f69d80c90a665fc9a1cf9
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C72B) = Uanis(C72)
Uanis(C73) = Uanis(C73B)
Uanis(O2B) = Uanis(O2)
3. Others
 Sof(O2B)=Sof(H71C)=Sof(H71D)=Sof(C72B)=Sof(H72C)=Sof(H72D)=Sof(C73B)=
 Sof(H73C)=Sof(H73D)=Sof(H74C)=Sof(H74D)=1-FVAR(1)
 Sof(O2)=Sof(H71A)=Sof(H71B)=Sof(C72)=Sof(H72A)=Sof(H72B)=Sof(C73)=Sof(H73A)=
 Sof(H73B)=Sof(H74A)=Sof(H74B)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C16(H16), C19(H19), C28(H28), C31(H31), C49(H49), C52(H52), C61(H61), C64(H64)
4.b Secondary CH2 refined with riding coordinates:
 C67(H67A,H67B), C68(H68A,H68B), C69(H69A,H69B), C70(H70A,H70B), C71(H71C,
 H71D), C71(H71A,H71B), C72(H72A,H72B), C72B(H72C,H72D), C73(H73A,H73B),
 C73B(H73C,H73D), C74(H74A,H74B), C74(H74C,H74D)
4.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13), C14(H14),
 C24(H24), C25(H25), C26(H26), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42),
  C45(H45), C46(H46), C47(H47), C57(H57), C58(H58), C59(H59)
4.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C53(H53A,H53B,H53C),
 C54(H54A,H54B,H54C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C65(H65A,H65B,
 H65C), C66(H66A,H66B,H66C)
;
_shelx_res_checksum              20349
_shelx_hkl_checksum              67159
_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 2.176
_oxdiff_exptl_absorpt_empirical_full_min 0.591
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2